CN104906144B

CN104906144B - Bioactive substance isolates and purifies Process Control System and method

Info

Publication number: CN104906144B
Application number: CN201510258549.5A
Authority: CN
Inventors: 王振宇; 李辉; 伊娟娟
Original assignee: Harbin Institute of Technology
Current assignee: Harbin Institute of Technology
Priority date: 2015-05-20
Filing date: 2015-05-20
Publication date: 2019-03-01
Anticipated expiration: 2035-05-20
Also published as: CN104906144A

Abstract

The invention discloses a kind of bioactive substances to isolate and purify Process Control System and method, and the system comprises extraction kettle, heater, heater hot water storage tank, surge tank, solvent recovery tank, inspissator, inspissator solvent recovery tank, concentration storage tank, chromatographic column, High Purity horizontal tank, pure water tank, parsing tank, sour tanks, alkali tank, blend tank, solvent tank, low purifying horizontal tank, sewage treatment pot.It is carried out at normal temperature the present invention has the advantage that being totally separated purification process, solves the problems, such as product processing stability；Realize the continuous operation of large-scale production；It shortens and isolates and purifies the period, simplified operation difficulty；Reduce product processing cost；Improve product quality；Solves sewage handling problem.

Description

Bioactive substance isolates and purifies Process Control System and method

Technical field

The invention belongs to automation control areas, are related to a kind of pair of bioactive substance and isolate and purify what process was controlled System and method.

Background technique

Modern society, bioactive substance is due to anti-oxidant, whitening, antitumor, adjusting immunity, anti-inflammatory, drop The bioactivity such as blood lipid, blood pressure lowering, anti-cardiovascular disease and anti-neurological disease, are with a wide range of applications, are usually used in Significant contribution is made to human health in the fields such as food, drug, health care product and cosmetics.Bioactive substance is mainly derived from Natural plant and microbial resources needs just obtain the product of high value, still, present work by the process isolated and purified Industry field is also main to the separation of bioactive substance using intensive manual mode of operation, and production equipment falls behind, and technology contains Amount is not high, is unable to continuity operation, leads to low yield, low efficiency is at high cost, and a cycle time is long, stable product quality Difference, it is seriously polluted etc., it is not suitable for the demand of current social development.

Summary of the invention

In order to solve bioactive substance isolate and purify in be unable to continuity operation, lead to low yield, low efficiency, cost The problems such as height, a cycle time is long, seriously polluted, and stable product quality is poor, and the degree of automation is low, the present invention provides one Kind bioactive substance isolates and purifies Process Control System and method.

The purpose of the present invention is what is be achieved through the following technical solutions:

A kind of bioactive substance isolates and purifies Process Control System, including the storage of extraction kettle, heater, heater hot water It is tank, surge tank, solvent recovery tank, inspissator, inspissator solvent recovery tank, concentration storage tank, chromatographic column, High Purity horizontal tank, pure Water pot, parsing tank, sour tank, alkali tank, blend tank, solvent tank, low purifying horizontal tank, sewage treatment pot, in which:

Mixing pump P9 and supersonic generator are installed, the feed inlet of extraction kettle is through Unidirectional solenoid valve S1 and certainly on extraction kettle Carry out water pipe connection, discharge port is connect with the feed inlet of downcomer and surge tank respectively through bidirectional electromagnetic valve D1, the bi-directional electromagnetic Infusion pump P5, bidirectional electromagnetic valve DS5 are sequentially installed on pipeline between valve D1 and feed inlet；

The feed inlet of surge tank is connect through bidirectional electromagnetic valve DS5 with running water pipe, and discharge port is distinguished through bidirectional electromagnetic valve D2 It connect, is sequentially installed on the pipeline between the bidirectional electromagnetic valve D2 and feed inlet defeated with the feed inlet of downcomer and inspissator Liquid pump P2, bidirectional electromagnetic valve D3；

Feed inlet of the discharge port of inspissator through three-way solenoid valve D4 respectively with downcomer, concentration liquid pipe, concentration storage tank connects It connects, infusion pump P3, bidirectional electromagnetic valve D23, unidirectional is sequentially installed on the pipeline between the three-way solenoid valve D4 and feed inlet Solenoid valve S13；Inspissator hot water outlet through Unidirectional solenoid valve S7, bidirectional electromagnetic valve D26 respectively with heater hot water storage tank and Jia Hot device connection, the outlet of heater hot water storage tank is connect through Unidirectional solenoid valve S50 with downcomer；

Inspissator solvent recovery tank upper end is condenser system, and condenser pipe import passes through Unidirectional solenoid valve S11 and condenser pipe Connection, condenser pipe outlet are connect by Unidirectional solenoid valve S10 with downcomer, and inspissator solvent recovery tank discharge port is through three-dimensional electromagnetism Valve D5 is connect with downcomer, concentration liquid pipe and recycling design pipe respectively, is pacified on the three-way solenoid valve D5 and recycling design pipeline Equipped with infusion pump P3 and bidirectional electromagnetic valve D23；

The water inlet of heater is connect through Unidirectional solenoid valve S2 with running water pipe, water outlet respectively with bidirectional electromagnetic valve D26 It is connected with inspissator, Unidirectional solenoid valve S3 is installed on the pipeline between the water outlet and inspissator；

The feed inlet of concentration storage tank is connect through Unidirectional solenoid valve S12 with running water pipe, and discharge port is through bidirectional electromagnetic valve D6 points Do not connect with the feed inlet of downcomer and chromatographic column, on the pipeline between the bidirectional electromagnetic valve D6 and the feed inlet of chromatographic column according to It is secondary that infusion pump P4, bidirectional electromagnetic valve D20, Unidirectional solenoid valve are installed；

A Unidirectional solenoid valve is connected at the feed inlet of chromatographic column, Unidirectional solenoid valve is connect with bidirectional electromagnetic valve D20, two-way Solenoid valve D20 is connect with downcomer, and the discharge port of chromatographic column is divided into water outlet and eluent outlet, and water outlet connects a list To solenoid valve, one bidirectional electromagnetic valve of eluent outlet connection, the eluent outlet of chromatographic column through bidirectional electromagnetic valve respectively with height Purifying horizontal tank is connected with low purifying horizontal tank feed inlet, is pacified on the pipeline between the bidirectional electromagnetic valve and low purifying horizontal tank Equipped with bidirectional electromagnetic valve D25；The water outlet of chromatographic column is connected through the feed inlet of Unidirectional solenoid valve and sewage treatment pot；

The feed inlet of sewage treatment pot is connect through Unidirectional solenoid valve S23 with running water pipe, and discharge port is through Unidirectional solenoid valve S24 It is connect with downcomer；

The feed inlet of High Purity horizontal tank is connect through Unidirectional solenoid valve S22 with running water pipe, and discharge port is through bidirectional electromagnetic valve D12 is connect with downcomer and infusion pump P5 respectively, and infusion pump P5 is connect with bidirectional electromagnetic valve D3；

The feed inlet of low purifying horizontal tank is connect through Unidirectional solenoid valve S37 with running water pipe, and discharge port is through bidirectional electromagnetic valve D13 is connect with downcomer and infusion pump P6 respectively, and infusion pump P6 is connect with bidirectional electromagnetic valve D3；

The feed inlet of pure water tank is connect through Unidirectional solenoid valve S25 with running water pipe, discharge port through pipeline respectively with downcomer It is connected with the Unidirectional solenoid valve of chromatographic column, is sequentially installed with bi-directional electromagnetic on the pipeline between the discharge port and Unidirectional solenoid valve Valve D14, infusion pump P7, Unidirectional solenoid valve S20, downcomer are connect with bidirectional electromagnetic valve D14；

The feed inlet of parsing tank is connect through Unidirectional solenoid valve S26 with running water pipe, and discharge port is distinguished through bidirectional electromagnetic valve D15 It is connect with infusion pump P7 and downcomer；

The feed inlet of sour tank is connect through Unidirectional solenoid valve S28 with running water pipe, discharge port through bidirectional electromagnetic valve D16 respectively with Infusion pump P7 is connected with downcomer；

The feed inlet of alkali tank is connect through Unidirectional solenoid valve S30 with running water pipe, discharge port through bidirectional electromagnetic valve D17 respectively with Infusion pump P7 is connected with downcomer；

The discharge port of blend tank is connect with infusion pump P8 and running water pipe respectively by bidirectional electromagnetic valve D18, infusion pump P8 It is connect respectively with the feed inlet of Unidirectional solenoid valve S1 and parsing tank, sour tank, alkali tank through bidirectional electromagnetic valve D24, the bi-directional electromagnetic Unidirectional solenoid valve S27, bidirectional electromagnetic valve D24 and sour tank feed inlet are installed on the pipeline between valve D24 and parsing tank feed inlet Between pipeline on Unidirectional solenoid valve S29 is installed, list is installed on the pipeline between bidirectional electromagnetic valve D24 and alkali tank feed inlet To solenoid valve S31；

The feed inlet of solvent recovery tank is connect with running water pipe and recycling design pipe respectively through pipeline, and discharge port is through two-way electricity Magnet valve D22 is connect with downcomer and infusion pump P10 respectively, infusion pump P10 through pipeline respectively with blend tank and solvent tank into Material mouth connection, described, the pipeline connection between bidirectional electromagnetic valve D21 and infusion pump P8 and bidirectional electromagnetic valve D24, the infusion pump Bidirectional electromagnetic valve DK is installed on the pipeline between P10 and solvent tank；

The feed inlet of solvent tank is connect through Unidirectional solenoid valve S33 with running water pipe, and discharge port is through bidirectional electromagnetic valve D19 points Pipeline not between downcomer, infusion pump P8 and bidirectional electromagnetic valve D18 is connect.

A method of bioactive substance is carried out using above-mentioned control system and isolates and purifies process control, including following several A process:

One, extraction process:

Step 1: starting bidirectional electromagnetic valve D18(0,2), infusion pump P8, bidirectional electromagnetic valve D24(0,1) and Unidirectional solenoid valve S1, after solvent enters 100~120L in extraction kettle, close bidirectional electromagnetic valve D18(0,2), infusion pump P8, bidirectional electromagnetic valve D24(0,1) and Unidirectional solenoid valve S1；

Step 2: starting infusion pump P9, supersonic generator continuous extraction bioactive substance 30~60 minutes, are closed Infusion pump P9, supersonic generator；

Step 3: starting bidirectional electromagnetic valve D1(0,2), infusion pump P1 and bidirectional electromagnetic valve DS5(2,1), when extracting solution into Enter in surge tank after 100~120L, close bidirectional electromagnetic valve D1(0,2), infusion pump P1 and bidirectional electromagnetic valve DS5(2,1)；

Step 4: step 1~3 1 time are repeated；

Two, concentration process:

Step 1: starting Unidirectional solenoid valve S2 closes Unidirectional solenoid valve S2 into heater plus after 150~200L of water；

Step 2: starting heater, heater hot water storage tank, water temperature are controlled at 50~60 DEG C；

Step 3: starting bidirectional electromagnetic valve D2(0,2), infusion pump P2, bidirectional electromagnetic valve D3(1,0), 100~120L extracts After liquid enters in inspissator, close bidirectional electromagnetic valve D2(0,2), infusion pump P2, bidirectional electromagnetic valve D3(1,0), start inspissator, When extracting solution is concentrated into 30~50L, inspissator is closed；

Step 4: open three-way solenoid valve D4(0,2), and Unidirectional solenoid valve infusion pump P3, bidirectional electromagnetic valve D23(0,1) S13, when concentrate enter concentration storage tank in 30~40L after, close three-way solenoid valve D4(0,2), infusion pump P3, bidirectional electromagnetic valve And Unidirectional solenoid valve S13 D23(0,1)；

Step 5: open bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2), returned when entering solvent When recycling design in closed cans is 50~100L, close bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0, 2)；

Three, purification process:

Step 1: open bidirectional electromagnetic valve D6(0,2), infusion pump P4, bidirectional electromagnetic valve D20(1,0)；Open unidirectional electromagnetism Valve, each chromatography column volume that control concentrate enters chromatographic column is 8L, closes valve when reaching 8L, when entirely reaching 8L, Close bidirectional electromagnetic valve D6(0,2), infusion pump P4, bidirectional electromagnetic valve D20(1,0)；

Step 2: open bidirectional electromagnetic valve D14(0,2), infusion pump P7, Unidirectional solenoid valve S20, bidirectional electromagnetic valve D25(0, 2)；Unidirectional solenoid valve is opened, is discharged bidirectional electromagnetic valve (0,2), is 64~96L by Unidirectional solenoid valve control pure water inlet, Close valve when reaching 64~96L, when inlet entirely reaches 64~96L, close bidirectional electromagnetic valve D14(0,2), two-way electricity Magnet valve D25(0,2), while flow, 10~32L/h of flow-control scope are controlled by water outlet bidirectional electromagnetic valve；

Step 3: as bidirectional electromagnetic valve D14(0,2) close when, starting bidirectional electromagnetic valve D15(0,2), bidirectional electromagnetic valve D25(0,1), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve, water outlet bidirectional electromagnetic valve (0,2) are in starting shape at this time State controls flow by water outlet bidirectional electromagnetic valve and concentration is converted, flow-control scope: 10~32L/h, when any chromatography post detection When to high concentration, bidirectional electromagnetic valve valve is discharged by (0,2) state and is converted to (0,1) state, while opening Unidirectional solenoid valve S21；When any chromatography post detection is to when becoming low concentration again from high concentration, water outlet bidirectional electromagnetic valve is converted to by (0,1) state (0,2) state, simultaneously closes off Unidirectional solenoid valve S21；

Step 4: when refined solution reaches 150~160L in High Purity horizontal tank, open bidirectional electromagnetic valve D12(0,2), Infusion pump P5, bidirectional electromagnetic valve D3, into inspissator, when flow reaches 150~160L, closing bidirectional electromagnetic valve D12(0, 2), infusion pump P5, two-way to solenoid valve D5, prepares starting inspissator；

Step 5: according to concentration step one and two, starting inspissator, when high-purity eluent is concentrated into 15~30L, closes Close inspissator, starting three-way solenoid valve D4(0,3) collects high-purity concentrate；

Step 6: open bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2), when recycling design is complete When portion enters in solvent recovery tank, close bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2)；

Four, solvent recovery process:

Step 1: after High Purity liquid is concentrated, step four~six in purification process is repeated, low refined solution solvent is carried out Recycling prepares；

Step 2: low-purity chromatographic solution in low purifying horizontal tank is put into inspissator, starting bidirectional electromagnetic valve D13 (0, 2), infusion pump P6, bidirectional electromagnetic valve D3(0,1) are closed after the emptying of low purifying horizontal tank；The step of repeating two, concentration process One, to step 5, obtains low pure concentrate；It opens three-way solenoid valve D4(0,1) by low pure concentrate taking-up, closes three-dimensional after taking-up Solenoid valve D4；

Step 3: when recycling design is close to maximum volume in inspissator solvent recovery tank, starting bidirectional electromagnetic valve D5(0, 1), infusion pump P3, bidirectional electromagnetic valve D23(0,2), after emptying, close bidirectional electromagnetic valve D5(0,1), infusion pump P3, bi-directional electromagnetic Valve D23(0,2)；

Step 4: when recycling amount of alcohol reaches maximum volume in solvent recovery tank 4, starting bidirectional electromagnetic valve D22(0, 2), mixing pump P9, bidirectional electromagnetic valve Dk(0,2)；

Five, activation process:

Step 1: starting Unidirectional solenoid valve S19, Unidirectional solenoid valve, water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49, one is small Shi Hou closes Unidirectional solenoid valve S19, Unidirectional solenoid valve, water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49 respectively；

Step 2: starting bidirectional electromagnetic valve D14(0,2), infusion pump P7, Unidirectional solenoid valve S20, inflow reaches in chromatographic column When 16~32L close bidirectional electromagnetic valve D14(0,2), infusion pump P7, Unidirectional solenoid valve S20；After 6~8 hours, starting water outlet is single Water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49 are closed to solenoid valve, Unidirectional solenoid valve S49, after emptying；

Step 3: starting bidirectional electromagnetic valve D16(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve, enter When acid intake amount reaches 16~32L in sewage treatment pot 17, chromatographic column, close bidirectional electromagnetic valve D16(0,2), it is infusion pump P7, unidirectional Solenoid valve S20, Unidirectional solenoid valve；After 6~8 hours, starting water outlet Unidirectional solenoid valve closes water outlet Unidirectional solenoid valve after emptying；

Step 4: starting Unidirectional solenoid valve S19, Unidirectional solenoid valve, water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49, two is small Shi Hou closes Unidirectional solenoid valve S19 respectively, water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49 is closed after tap water emptying；

Step 5: starting bidirectional electromagnetic valve D17(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve, chromatography When reaching 16~32L into alkali number in column, close bidirectional electromagnetic valve D17(0,2), infusion pump P7, Unidirectional solenoid valve S20, unidirectional electricity Magnet valve；After 6~8 hours, starting water outlet Unidirectional solenoid valve closes water outlet Unidirectional solenoid valve after emptying into sewage treatment pot；

Step 6: starting Unidirectional solenoid valve S19, Unidirectional solenoid valve, water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49, two is small Shi Hou closes Unidirectional solenoid valve S19, water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49 is closed after tap water emptying；

Step 7: starting bidirectional electromagnetic valve D15(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve, chromatography When column internal solvent input reaches 16~32L, close bidirectional electromagnetic valve D15(0,2), it is infusion pump P7, Unidirectional solenoid valve S20, unidirectional Solenoid valve, it is stand-by；Next time is put into low purifying horizontal tank before purification, by solvent, opens water outlet bidirectional electromagnetic valve (0,2), double To solenoid valve D25(0,1)；

Six, allocation process:

1, desorbed solution is deployed: starting bidirectional electromagnetic valve D19(0,2), infusion pump P8, bidirectional electromagnetic valve D21(1,2), enter Measure 50~200L, starting bidirectional electromagnetic valve D22(0,2), mixing pump P9, bidirectional electromagnetic valve D21(0,2), 50~200L of inlet, Start Unidirectional solenoid valve S32,50~200L of inlet, starting stirring 30 minutes；

2, acid solution is prepared: starting Unidirectional solenoid valve S32,50~200L of inlet, acid liquid, starting stirring 30 minutes；

3, Alkali liquid compounding: alkali piece, starting stirring 40 minutes is added in starting Unidirectional solenoid valve S32,50~200L of inlet；

4, pure water: starting Unidirectional solenoid valve S25, inlet 300L；

Seven, cleaning process:

1, extraction kettle: starting Unidirectional solenoid valve S1 after reaching maximum volume, is closed；After impregnating 12 hours, start bi-directional electromagnetic Valve D1 (0,1) is closed all after emptying；It is again started up Unidirectional solenoid valve S1, after reaching maximum volume, closes Unidirectional solenoid valve S1, bidirectional electromagnetic valve D1 (0,1) is opened, all after emptying, closed, cleaning terminates；

2, extraction kettle, heater, heater hot water storage tank, surge tank, solvent recovery tank, inspissator, inspissator solvent return It is closed cans, concentration storage tank, chromatographic column, High Purity horizontal tank, pure water tank, parsing tank, sour tank, alkali tank, blend tank, solvent tank, low Purify horizontal tank, sewage treatment pot presses extraction kettle cleaning method.

In the present invention, the bioactive substance includes polyphenol, flavones, anthocyanin, procyanidine, saponin, alkaloid, more The bioactive substances such as sugar, protein, enzyme, amino acid, polypeptide, pigment.

In the present invention, in the extraction process, extractant accounts for the 1/2~3/4 of extraction kettle total volume, solid-liquid ratio 1:5 ~20, the combining extraction liquid once and twice extracted accounts for the 1/2~3/4 of surge tank total volume.

In the present invention, in the concentration process, extracting liquid volume accounts for the 1/4~1/2 of inspissator total volume, is concentrated to substance Long-pending 1/3~1/5 or so.

In the present invention, in the purification process, the volume of the concentrated liquid accounts for the 1/4~1/5 of column volume, and pure water consumption is 2~4 A column volume, eluent dosage are 2~4 column volumes, and elution flow rate is 0.1~1 column volume/h, and chromatographic column quantity is 4~30.

In the present invention, in the solvent recovery process, low-purity eluent only carries out solvent recovery, extracting solution and extract liquor Concentration and solvent recovery are carried out simultaneously.

In the present invention, in the activation process, acid solution dosage is 1.5~1 column volumes, and aqueous slkali dosage is 1.5~1 A column volume.

In the present invention, in the allocation process, 40~80%(v/v of concentration of desorbed solution), the concentration of acid solution is 1~5% (w/v), the concentration of aqueous slkali is 1~5%(w/v).

It, water cleaning equipment 2 times, can be with into progress to the cleaning of equipment in the cleaning process in the present invention.

The present invention has the advantage that

1, it is totally separated purification process to carry out at normal temperature, solves the problems, such as product processing stability；

2, the continuous operation of large-scale production is realized；

3, it shortens and isolates and purifies the period, simplified operation difficulty；

4, product processing cost is reduced；

5, product quality is improved；

6, sewage handling problem is solved.

Detailed description of the invention

Fig. 1 is that bioactive substance isolates and purifies process control schematic diagram；

Fig. 2 is partial enlarged view at the A of Fig. 1；

Fig. 3 is partial enlarged view at the B of Fig. 1；

Fig. 4 is partial enlarged view at the C of Fig. 1；

Fig. 5 is partial enlarged view at the D of Fig. 1；

Fig. 6 is partial enlarged view at the E of Fig. 1；

Fig. 7 is partial enlarged view at the F of Fig. 1.

Specific embodiment

Further description of the technical solution of the present invention with reference to the accompanying drawing, and however, it is not limited to this, all to this Inventive technique scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered Within the protection scope of the present invention.

Specific embodiment 1: as shown in figs. 1-7, bioactive substance described in present embodiment isolated and purified program-controlled System processed includes extraction kettle 1, heater 2, heater hot water storage tank 2-1, surge tank 3, solvent recovery tank 4, inspissator 5, concentration Device solvent recovery tank 5-1, concentration storage tank 6, chromatographic column 7, High Purity horizontal tank 8, condenser system 9, pure water tank 10, parsing tank 11, Sour tank 12, alkali tank 13, blend tank 14, solvent tank 15, low purifying horizontal tank 16, infusion pump, control valve, sewage treatment pot 17. It is connected by pipeline with control valve between each equipment according to process control, specific connection relationship is as follows:

Mixing pump P9 and supersonic generator be installed on extraction kettle 1, the feed inlet of extraction kettle 1 through Unidirectional solenoid valve S1 with Running water pipe connection, discharge port are connect with the feed inlet of downcomer and surge tank 3 respectively through bidirectional electromagnetic valve D1, the two-way electricity Infusion pump P5, bidirectional electromagnetic valve DS5 are sequentially installed on pipeline between magnet valve D1 and feed inlet；

The feed inlet of surge tank 3 is connect through bidirectional electromagnetic valve DS5 with running water pipe, and discharge port is distinguished through bidirectional electromagnetic valve D2 It connect with the feed inlet of downcomer and inspissator 5, is sequentially installed on the pipeline between the bidirectional electromagnetic valve D2 and feed inlet Infusion pump P2, bidirectional electromagnetic valve D3；

The discharge port of inspissator 5 through three-way solenoid valve D4 respectively with downcomer, concentration liquid pipe, be concentrated storage tank 6 feed inlet It connects, is sequentially installed with infusion pump P3, bidirectional electromagnetic valve D23, list on the pipeline between the three-way solenoid valve D4 and feed inlet To solenoid valve S13；5 hot water outlet of inspissator through Unidirectional solenoid valve S7, bidirectional electromagnetic valve D26 respectively with heater hot water storage tank 2- 1 and heater 2 connect, the outlet of heater hot water storage tank 2-1 is connect through Unidirectional solenoid valve S50 with downcomer；

The inspissator upper end solvent recovery tank 5-1 be condenser system 9, condenser pipe import by Unidirectional solenoid valve S11 with it is cold Solidifying pipe connection, condenser pipe outlet are connect by Unidirectional solenoid valve S10 with downcomer, inspissator solvent recovery tank 5-1 discharge port warp Three-way solenoid valve D5 is connect with downcomer, concentration liquid pipe and recycling design pipe respectively, the three-way solenoid valve D5 and recycling design Infusion pump P3 and bidirectional electromagnetic valve D23 are installed on pipeline；

The water inlet of heater 2 is connect through Unidirectional solenoid valve S2 with running water pipe, water outlet respectively with bidirectional electromagnetic valve D26 It is connected with inspissator 5, Unidirectional solenoid valve S3 is installed on the pipeline between the water outlet and inspissator 5；

The feed inlet of concentration storage tank 6 is connect through Unidirectional solenoid valve S12 with running water pipe, and discharge port is through bidirectional electromagnetic valve D6 points It is not connect with the feed inlet of downcomer and chromatographic column 7, on the pipeline between the bidirectional electromagnetic valve D6 and the feed inlet of chromatographic column 7 It is sequentially installed with infusion pump P4, bidirectional electromagnetic valve D20, Unidirectional solenoid valve；

The quantity of chromatographic column 7 is 4, connects a Unidirectional solenoid valve (that is: S14~S17) at the feed inlet of each chromatographic column, Unidirectional solenoid valve S14~S17 is connect with bidirectional electromagnetic valve D20, and bidirectional electromagnetic valve D20 is connect with downcomer, each chromatographic column Discharge port is divided into water outlet and eluent outlet, and water outlet connects a water outlet Unidirectional solenoid valve (that is: S44~S47), elution One water outlet bidirectional electromagnetic valve (that is: D7~D10) of liquid outlet connection.The eluent outlet of chromatographic column 7 is through being discharged bidirectional electromagnetic valve D7~D10 is connect with High Purity horizontal tank 8 and low 16 feed inlet of purifying horizontal tank respectively, the bidirectional electromagnetic valve D7~D10 with Bidirectional electromagnetic valve D25 is installed on pipeline between low purifying horizontal tank 16；The water outlet of chromatographic column 7 is through Unidirectional solenoid valve S44 ~S47, Unidirectional solenoid valve S48 are connect with the feed inlet of sewage treatment pot 17；

The feed inlet of sewage treatment pot 17 is connect through Unidirectional solenoid valve S23 with running water pipe, and discharge port is through Unidirectional solenoid valve S24 is connect with downcomer；

The feed inlet of High Purity horizontal tank 8 is connect through Unidirectional solenoid valve S22 with running water pipe, and discharge port is through bidirectional electromagnetic valve D12 is connect with downcomer and infusion pump P5 respectively, and infusion pump P5 is connect with bidirectional electromagnetic valve D3；

The feed inlet of low purifying horizontal tank 16 is connect through Unidirectional solenoid valve S37 with running water pipe, and discharge port is through bi-directional electromagnetic Valve D13 is connect with downcomer and infusion pump P6 respectively, and infusion pump P6 is connect with bidirectional electromagnetic valve D3；

The feed inlet of pure water tank 10 is connect through Unidirectional solenoid valve S25 with running water pipe, discharge port through pipeline respectively be lauched Pipe is connected with Unidirectional solenoid valve S14~S17 of chromatographic column 7, the pipeline between the discharge port and Unidirectional solenoid valve S14~S17 On be sequentially installed with bidirectional electromagnetic valve D14, infusion pump P7, Unidirectional solenoid valve S20, downcomer is connect with bidirectional electromagnetic valve D14；

The feed inlet of parsing tank 11 is connect through Unidirectional solenoid valve S26 with running water pipe, and discharge port is through bidirectional electromagnetic valve D15 points It is not connect with infusion pump P7 and downcomer；

The feed inlet of sour tank 12 is connect through Unidirectional solenoid valve S28 with running water pipe, and discharge port is distinguished through bidirectional electromagnetic valve D16 It is connect with infusion pump P7 and downcomer；

The feed inlet of alkali tank 13 is connect through Unidirectional solenoid valve S30 with running water pipe, and discharge port is distinguished through bidirectional electromagnetic valve D17 It is connect with infusion pump P7 and downcomer；

The discharge port of blend tank 14 is connect with infusion pump P8 and running water pipe respectively by bidirectional electromagnetic valve D18, infusion pump P8 is connect with the feed inlet of Unidirectional solenoid valve S1 and parsing tank 11, sour tank 12, alkali tank 13 respectively through bidirectional electromagnetic valve D24, described Unidirectional solenoid valve S27 is installed on pipeline between bidirectional electromagnetic valve D24 and parsing 11 feed inlet of tank, bidirectional electromagnetic valve D24 with Unidirectional solenoid valve S29 is installed, between 13 feed inlet of bidirectional electromagnetic valve D24 and alkali tank on the pipeline between sour 12 feed inlet of tank Unidirectional solenoid valve S31 is installed on pipeline；

The feed inlet of solvent recovery tank 4 is connect with running water pipe and recycling design pipe respectively through pipeline, and discharge port is through two-way Solenoid valve D22 is connect with downcomer and infusion pump P10 respectively, infusion pump P10 through pipeline respectively with blend tank 14 and solvent tank 15 feed inlet connection, described, the pipeline connection between bidirectional electromagnetic valve D21 and infusion pump P8 and bidirectional electromagnetic valve D24 are described Bidirectional electromagnetic valve DK is installed on the pipeline between infusion pump P10 and solvent tank 15；

The feed inlet of solvent tank 15 is connect through Unidirectional solenoid valve S33 with running water pipe, and discharge port is through bidirectional electromagnetic valve D19 The pipeline between downcomer, infusion pump P8 and bidirectional electromagnetic valve D18 is connect respectively.

Control valve is the unidirectional and bidirectional electromagnetic valve for automation control, and wherein D1~D31, DK and DS are bi-directional electromagnetic Valve, S1~S35 are Unidirectional solenoid valve, and D4 is enrichment control valve and three-way pilot valve, and D7~D10 is flow control and sweetness degree Switching valve, S34, S14~S19 are flow control valve, and D12~D13 is capacity control drive.

Present embodiment shares following process: one, extraction process: extract bioactive substance from raw material, two, dense Compression process: three, purification process: the bioactive substance of concentrated extract and eluent isolates and purifies life from extraction concentrate Four, solvent recovery process: active substances recycle organic solvent, five, activation process from extract liquor and eluent: activation and Separating medium is regenerated, six, allocation process: preparing eluent and acid, aqueous slkali, seven, cleaning process: clean all equipment and pipe Road, in case application next time.Detailed process control are as follows:

One, extraction process:

Step 1: starting bidirectional electromagnetic valve D18(0,2), infusion pump P8, bidirectional electromagnetic valve D24(0,1) and Unidirectional solenoid valve S1, after solvent enters 100~120L in extraction kettle 1, close bidirectional electromagnetic valve D18(0,2), infusion pump P8, bidirectional electromagnetic valve D24(0,1) and Unidirectional solenoid valve S1.

Step 2: starting infusion pump P9, supersonic generator continuous extraction 30~60 minutes, close infusion pump P9, ultrasound Wave producer.

Step 3: starting bidirectional electromagnetic valve D1(0,2), infusion pump P1 and bidirectional electromagnetic valve DS5(2,1), when extracting solution into Enter in surge tank 3 after 100~120L, close bidirectional electromagnetic valve D1(0,2), infusion pump P1 and bidirectional electromagnetic valve DS5(2,1).

Step 4: step 1~3 1 time are repeated.

Two, concentration process:

Step 1: starting Unidirectional solenoid valve S2 closes Unidirectional solenoid valve S2 into heater 2 plus after 150~200L of water.

Step 2: starting heater 2, heater hot water storage tank 2-1, water temperature are controlled at 50~60 DEG C.

Step 3: starting bidirectional electromagnetic valve D2(0,2), infusion pump P2, bidirectional electromagnetic valve D3(1,0), 100~120L extracts After liquid enters in inspissator 5, close bidirectional electromagnetic valve D2(0,2), infusion pump P2, bidirectional electromagnetic valve D3(1,0), start inspissator 5, when extracting solution is concentrated into 30~50L, close inspissator 5.

Step 4: open three-way solenoid valve D4(0,2), and Unidirectional solenoid valve infusion pump P3, bidirectional electromagnetic valve D23(0,1) S13, when concentrate enter concentration storage tank 6 in 30~40L after, close three-way solenoid valve D4(0,2), infusion pump P3, bi-directional electromagnetic And Unidirectional solenoid valve S13 valve D23(0,1).

Step 5: open bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2), returned when entering solvent When recycling design in closed cans 4 is 50~100L, close bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0, 2).

Three, purification process:

Step 1: open bidirectional electromagnetic valve D6(0,2), infusion pump P4, bidirectional electromagnetic valve D20(1,0)；Open unidirectional electromagnetism Valve S14~S17, it is 8L that each valve control concentrate, which enters each chromatography column volume of chromatographic column 7, closes valve when reaching 8L Door, when each valve of Unidirectional solenoid valve S14~S17 entirely reaches 8L, close bidirectional electromagnetic valve D6(0,2), it is infusion pump P4, two-way Solenoid valve D20(1,0).

Step 2: open bidirectional electromagnetic valve D14(0,2), infusion pump P7, Unidirectional solenoid valve S20, bidirectional electromagnetic valve D25(0, 2)；Unidirectional solenoid valve S14~S17, bidirectional electromagnetic valve D7~D10(0,2) are opened, is controlled and is intake by Unidirectional solenoid valve S14~S17 Amount, each valve control pure water inlet be 64~96L, close valve when reaching 64~96L, when Unidirectional solenoid valve S14~ When each valve inlet of S17 entirely reaches 64~96L, close bidirectional electromagnetic valve D14(0,2), bidirectional electromagnetic valve D25(0,2).Together When by bidirectional electromagnetic valve D7~D10 control flow, 10~32L/h of flow-control scope.

Step 3: as bidirectional electromagnetic valve D14(0,2) close when, starting bidirectional electromagnetic valve D15(0,2), bidirectional electromagnetic valve D25(0,1), at this time infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~S17, bidirectional electromagnetic valve D7~D10(0,2) In starting state.Flow and concentration (sweet spot) conversion are controlled by bidirectional electromagnetic valve D7~D10, flow-control scope: 10~ 32L/h, when chromatography post detection any in bidirectional electromagnetic valve D7~D10 is to high concentration, which is converted to by (0,2) state (0,1) state, while opening Unidirectional solenoid valve S21.When chromatography post detection any in bidirectional electromagnetic valve D7~D10 is to by high concentration When becoming low concentration again, which is converted to (0,2) state by (0,1) state, simultaneously closes off Unidirectional solenoid valve S21.

Step 4: when refined solution reaches 150~160L in High Purity horizontal tank 8, open bidirectional electromagnetic valve D12(0,2), Infusion pump P5, bidirectional electromagnetic valve D3, into inspissator 5, when flow reaches 150~160L, closing bidirectional electromagnetic valve D12(0, 2), infusion pump P5, two-way to solenoid valve D5, prepares starting inspissator 5.

Step 5: according to concentration step one and two, starting inspissator 5, when high-purity eluent is concentrated into 15~30L, Inspissator 5 is closed, starting three-way solenoid valve D4(0,3) collects high-purity concentrate.

Step 6: open bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2), when recycling design is complete When portion enters in solvent recovery tank 4, close bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2).

Four, solvent recovery process:

Step 1: after High Purity liquid is concentrated, step four~six in purification process is repeated, low refined solution solvent is carried out Recycling prepares.

Step 2: low-purity chromatographic solution in low purifying horizontal tank 16 is put into inspissator 5, starts bidirectional electromagnetic valve D13 (0,2), infusion pump P6, bidirectional electromagnetic valve D3(0,1), after the emptying of low purifying horizontal tank 16, close.Repeat two, concentration process The step of one to step 5, obtain low pure concentrate.It opens three-way solenoid valve D4(0,1) by low pure concentrate taking-up, is closed after taking-up Close three-way solenoid valve D4.

Step 3: when recycling design is close to maximum volume in inspissator solvent recovery tank 5-1, start bidirectional electromagnetic valve D5 (0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2), after emptying, close bidirectional electromagnetic valve D5(0,1), it is infusion pump P3, two-way Solenoid valve D23(0,2).

Step 4: when recycling design amount reaches maximum volume in solvent recovery tank 4, starting bidirectional electromagnetic valve D22(0, 2), mixing pump P9, bidirectional electromagnetic valve Dk(0,2).

Five, activation process:

Step 1: starting Unidirectional solenoid valve S19, Unidirectional solenoid valve S14~S17, Unidirectional solenoid valve S44~S47, unidirectional electricity Magnet valve S49, after one hour, respectively close Unidirectional solenoid valve S19, Unidirectional solenoid valve S14~S17, Unidirectional solenoid valve S44~S47, Unidirectional solenoid valve S49.

Step 2: starting bidirectional electromagnetic valve D14(0,2), infusion pump P7, Unidirectional solenoid valve S20, inflow in chromatographic column 7 Closed when up to 16~32L bidirectional electromagnetic valve D14(0,2), infusion pump P7, Unidirectional solenoid valve S20.After 6~8 hours, starting is unidirectional Solenoid valve S44~S47, Unidirectional solenoid valve S49 close Unidirectional solenoid valve S44~S47, Unidirectional solenoid valve S49 after emptying.

Step 3: starting bidirectional electromagnetic valve D16(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~ S17, into sewage treatment pot 17, chromatographic column 7 in acid intake amount when reaching 16~32L, close bidirectional electromagnetic valve D16(0,2), infusion Pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~S17.After 6~8 hours, start Unidirectional solenoid valve S44~S48, emptying Unidirectional solenoid valve S44~S48 is closed afterwards.

Step 4: starting Unidirectional solenoid valve S19, Unidirectional solenoid valve S14~S17, Unidirectional solenoid valve S44~S47, unidirectional electricity Magnet valve S49 after two hours, closes Unidirectional solenoid valve S19 respectively, closes Unidirectional solenoid valve S44~S47, list after tap water emptying To solenoid valve S49.

Step 5: starting bidirectional electromagnetic valve D17(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~ S17, when reaching 16~32L into alkali number in chromatographic column 7, close bidirectional electromagnetic valve D17(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~S17.After 6~8 hours, start Unidirectional solenoid valve S44~S48, is emptied into sewage treatment pot 17 Unidirectional solenoid valve S44~S48 is closed afterwards.

Step 6: starting Unidirectional solenoid valve S19, Unidirectional solenoid valve S14~S17, Unidirectional solenoid valve S44~S47, unidirectional electricity Magnet valve S49 after two hours, closes Unidirectional solenoid valve S19, Unidirectional solenoid valve S44~S47, unidirectional electricity is closed after tap water emptying Magnet valve S49.

Step 7: starting bidirectional electromagnetic valve D15(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~ S17, when chromatographic column internal solvent input reaches 16~32L, close bidirectional electromagnetic valve D15(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~S17.It is stand-by.Next time is put into low purifying horizontal tank 16 before purification, by solvent, opens two-way Solenoid valve D7~D10(0,2), bidirectional electromagnetic valve D25(0,1).

Six, allocation process:

1, desorbed solution is deployed: starting bidirectional electromagnetic valve D19(0,2), infusion pump P8, bidirectional electromagnetic valve D21(1,2), enter Measure 50~200L, starting bidirectional electromagnetic valve D22(0,2), mixing pump P9, bidirectional electromagnetic valve D21(0,2), 50~200L of inlet, Start Unidirectional solenoid valve S32,50~200L of inlet.Starting stirring 30 minutes.

2, acid solution is prepared: starting Unidirectional solenoid valve S32,50~200L of inlet, acid liquid, starting stirring 30 minutes.

3, Alkali liquid compounding: alkali piece, starting stirring 40 minutes is added in starting Unidirectional solenoid valve S32,50~200L of inlet.

4, pure water: starting Unidirectional solenoid valve S25, inlet 300L.

Seven, cleaning process:

1, extraction kettle 1: starting Unidirectional solenoid valve S1 after reaching maximum volume, is closed.After impregnating 12 hours, start two-way electricity Magnet valve D1 (0,1) is closed all after emptying.It is again started up Unidirectional solenoid valve S1, after reaching maximum volume, closes unidirectional electromagnetism Valve S1, bidirectional electromagnetic valve D1 (0,1) is opened, all after emptying, closed, cleaning terminates.

2, heater 2, heater hot water storage tank 2-1, surge tank 3, solvent recovery tank 4, inspissator 5, inspissator solvent return Closed cans 5-1, concentration storage tank 6, chromatographic column 7, High Purity horizontal tank 8, pure water tank 10, parsing tank 11, sour tank 12, alkali tank 13, allotment Tank 14, solvent tank 15, low purifying horizontal tank 16, sewage treatment pot 17 press 1 cleaning method of extraction kettle.

Specific embodiment 2: provide a specific case study on implementation in present embodiment, the extractant of use and wash Desolventizing is ethanol solution.

The extraction feed of present embodiment is the plant powder crushed.

The separating medium used in present embodiment is macroreticular resin.

The acid solution used in present embodiment is hydrochloric acid.

The alkali used in present embodiment is sodium hydroxide.

Present embodiment includes the entire series process that bioactive substance isolates and purifies.

Present embodiment includes following seven control processes:

One, extraction process:

Step 1: starting bidirectional electromagnetic valve D18(0,2), infusion pump P8, bidirectional electromagnetic valve D24(0,1) and Unidirectional solenoid valve S1, after solvent enters 100L in extraction kettle 1, close bidirectional electromagnetic valve D18(0,2), infusion pump P8, bidirectional electromagnetic valve D24(0, And Unidirectional solenoid valve S1 1).

Step 2: starting infusion pump P9, supersonic generator continuous extraction 40 minutes, close infusion pump P9, ultrasonic wave hair Raw device.

Step 3: starting bidirectional electromagnetic valve D1(0,2), infusion pump P1 and bidirectional electromagnetic valve DS5(2,1), when extracting solution into Enter in surge tank 3 after 100L, close bidirectional electromagnetic valve D1(0,2), infusion pump P1 and bidirectional electromagnetic valve DS5(2,1).

Step 4: step 1~3 1 time are repeated.

Two, concentration process:

Step 1: starting Unidirectional solenoid valve S2 closes Unidirectional solenoid valve S2 into heater 2 plus after water 150L.

Step 2: starting heater 2, hot water barrel 2-1, water temperature are controlled at 50 DEG C.

Step 3: starting bidirectional electromagnetic valve D2(0,2), infusion pump P2, bidirectional electromagnetic valve D3(1,0), extracting solution enters dense In contracting device 5 after 100L, close bidirectional electromagnetic valve D2(0,2), infusion pump P2, bidirectional electromagnetic valve D3(1,0), start inspissator 5, very Reciprocal of duty cycle is 0.075MPa, when extracting solution is concentrated into 30L, closes inspissator 5.

Step 4: open three-way solenoid valve D4(0,2), and Unidirectional solenoid valve infusion pump P3, bidirectional electromagnetic valve D23(0,1) S13, when concentrate enter concentration storage tank 6 in 30L after, close three-way solenoid valve D4(0,2), infusion pump P3, bidirectional electromagnetic valve D23 (0,1) and Unidirectional solenoid valve S13.

Step 5: open bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2), returned when entering solvent When recycling ethyl alcohol in closed cans 4 is 50L, close bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2).

Three, purification process:

Step 2: open bidirectional electromagnetic valve D14(0,2), infusion pump P7, Unidirectional solenoid valve S20, bidirectional electromagnetic valve D25(0, 2)；Unidirectional solenoid valve S14~S17, bidirectional electromagnetic valve D7~D10(0,2) are opened, is controlled and is intake by Unidirectional solenoid valve S14~S17 Amount, each valve control pure water inlet are 96L, valve are closed when reaching 96L, when each valve of Unidirectional solenoid valve S14~S17 When inlet entirely reaches 96L(, close bidirectional electromagnetic valve D14(0,2), bidirectional electromagnetic valve D25(0,2).Simultaneously by bi-directional electromagnetic Valve D7~D10 controls flow, flow control 10L/h.

Step 3: as bidirectional electromagnetic valve D14(0,2) close when, starting bidirectional electromagnetic valve D15(0,2), bidirectional electromagnetic valve D25(0,1), at this time infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~S17, bidirectional electromagnetic valve D7~D10(0,2) In starting state.Flow is controlled by bidirectional electromagnetic valve D7~D10 and concentration (sweet spot) is converted, flow control 10L/h, when When any chromatography post detection is to high concentration in bidirectional electromagnetic valve D7~D10, which is converted to (0,1) state by (0,2) state, Unidirectional solenoid valve S21 is opened simultaneously.When chromatography post detection any in bidirectional electromagnetic valve D7~D10 to being become low dense from high concentration again When spending, which is converted to (0,2) state by (0,1) state, simultaneously closes off Unidirectional solenoid valve S21.

Step 4: when refined solution reaches 150L in High Purity horizontal tank 8, open bidirectional electromagnetic valve D12(0,2), infusion Pump P5, bidirectional electromagnetic valve D3, into inspissator 5, when flow reaches 150L, close bidirectional electromagnetic valve D12(0,2), infusion pump It is P5, two-way to solenoid valve D5, prepare starting inspissator 5.

Step 5: according to concentration step one and two, starting inspissator 5, when high-purity eluent is concentrated into 15L, closes Inspissator 5.Start three-way solenoid valve D4(0,3), collects high-purity concentrate.

Step 6: open bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2), when recycling ethyl alcohol is complete When portion enters in solvent recovery tank 4, close bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2).

Four, solvent recovery:

Step 1: after High Purity liquid is concentrated, repeatedly the step five in purification process, six, carry out low refined solution solvent Recycling prepares.

Step 3: when recycling design is close to maximum volume in the solvent recovery tank 5-1 of inspissator, start bidirectional electromagnetic valve D5(0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2), after emptying, close bidirectional electromagnetic valve D5(0,1), it is infusion pump P3, double To solenoid valve D23(0,2).

Step 4: when recycling amount of alcohol reaches maximum volume in solvent recovery tank 4, starting bidirectional electromagnetic valve D22(0, 2), mixing pump P9, bidirectional electromagnetic valve Dk(0,2).

Five, activation process are as follows:

Step 2: starting bidirectional electromagnetic valve D14(0,2), infusion pump P7, Unidirectional solenoid valve S20, inflow in chromatographic column 7 Closed when up to 32L bidirectional electromagnetic valve D14(0,2), infusion pump P7, Unidirectional solenoid valve S20.After 6 hours, start Unidirectional solenoid valve S44~S47, Unidirectional solenoid valve S49 close Unidirectional solenoid valve S44~S47, Unidirectional solenoid valve S49 after emptying.

Step 3: starting bidirectional electromagnetic valve D16(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~ S17, into sewage treatment pot 17, chromatographic column 7 in acid intake amount when reaching 32L, close bidirectional electromagnetic valve D16(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~S17.After 6 hours, starts Unidirectional solenoid valve S44~S48, closed after emptying Unidirectional solenoid valve S44~S48.

Step 5: starting bidirectional electromagnetic valve D17(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~ S17, when reaching 32L into alkali number in chromatographic column 7, close bidirectional electromagnetic valve D17(0,2), infusion pump P7, Unidirectional solenoid valve S20, list To solenoid valve S14~S17.After 6 hours, start Unidirectional solenoid valve S44~S48, is closed after being emptied into sewage treatment pot 17 single To solenoid valve S44~S48.

Step 7: starting bidirectional electromagnetic valve D15(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~ S17, when ethyl alcohol input reaches 32L in chromatographic column, close bidirectional electromagnetic valve D15(0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve S14~S17.It is stand-by.Next time is put into low purifying horizontal tank 16 before purification, by ethyl alcohol, opens bi-directional electromagnetic Valve D7~D10(0,2), bidirectional electromagnetic valve D25(0,1).

Six, allocation process:

(1) desorbed solution deploy: starting bidirectional electromagnetic valve D19(0,2), infusion pump P8, bidirectional electromagnetic valve D21(1,2), enter Measure 100L, starting bidirectional electromagnetic valve D22(0,2), mixing pump P9, bidirectional electromagnetic valve D21(0,2), inlet 100L, starting is unidirectional Solenoid valve S32, inlet 100L.Starting stirring 30 minutes.

(2) acid solution is prepared: starting Unidirectional solenoid valve S32, inlet 200L, acid liquid, starting stirring 30 minutes.

(3) Alkali liquid compounding: alkali piece, starting stirring 40 minutes is added in starting Unidirectional solenoid valve S32, inlet 200L.

(4) pure water: starting Unidirectional solenoid valve S25, inlet 300L.

Seven, cleaning process:

(1) extraction kettle 1: starting Unidirectional solenoid valve S1 after reaching maximum volume, is closed.After impregnating 12 hours, start two-way electricity Magnet valve D1 (0,1) is closed all after emptying.It is again started up Unidirectional solenoid valve S1, after reaching maximum volume, closes unidirectional electromagnetism Valve S1, bidirectional electromagnetic valve D1 (0,1) is opened, all after emptying, closed, cleaning terminates.

(2) heater 2, heater hot water storage tank 2-1, surge tank 3, solvent recovery tank 4, inspissator 5, inspissator solvent return Closed cans 5-1, concentration storage tank 6, chromatographic column 7, High Purity horizontal tank 8, pure water tank 10, parsing tank 11, sour tank 12, alkali tank 13, allotment Tank 14, solvent tank 15, low purifying horizontal tank 16, sewage treatment pot 17 press 1 cleaning method of extraction kettle.

Claims

1. a kind of bioactive substance isolates and purifies Process Control System, it is characterised in that the system by extraction kettle, heater, It is heater hot water storage tank, surge tank, solvent recovery tank, inspissator, inspissator solvent recovery tank, concentration storage tank, chromatographic column, high-purity Change horizontal tank, pure water tank, parsing tank, sour tank, alkali tank, blend tank, solvent tank, low purifying horizontal tank, sewage treatment pot composition, Wherein:

Mixing pump P9 and supersonic generator are installed, the feed inlet of extraction kettle is through Unidirectional solenoid valve S1 and certainly on the extraction kettle Carry out water pipe connection, discharge port is connect with the feed inlet of downcomer and surge tank respectively through bidirectional electromagnetic valve D1, the bi-directional electromagnetic Infusion pump P5, bidirectional electromagnetic valve DS5 are sequentially installed on pipeline between valve D1 and feed inlet；

The feed inlet of the surge tank is connect through bidirectional electromagnetic valve DS5 with running water pipe, and discharge port is distinguished through bidirectional electromagnetic valve D2 It connect, is sequentially installed on the pipeline between the bidirectional electromagnetic valve D2 and feed inlet defeated with the feed inlet of downcomer and inspissator Liquid pump P2, bidirectional electromagnetic valve D3；

Feed inlet of the discharge port of the inspissator through three-way solenoid valve D4 respectively with downcomer, concentration liquid pipe, concentration storage tank connects It connects, infusion pump P3, bidirectional electromagnetic valve D23, unidirectional is sequentially installed on the pipeline between the three-way solenoid valve D4 and feed inlet Solenoid valve S13；Inspissator hot water outlet through Unidirectional solenoid valve S7, bidirectional electromagnetic valve D26 respectively with heater hot water storage tank and Jia Hot device connection, the outlet of heater hot water storage tank is connect through Unidirectional solenoid valve S50 with downcomer；

The water inlet of the heater is connect through Unidirectional solenoid valve S2 with running water pipe, water outlet respectively with bidirectional electromagnetic valve D26 It is connected with inspissator, Unidirectional solenoid valve S3 is installed on the pipeline between the water outlet and inspissator；

The feed inlet of the concentration storage tank is connect through Unidirectional solenoid valve S12 with running water pipe, and discharge port is through bidirectional electromagnetic valve D6 points Do not connect with the feed inlet of downcomer and chromatographic column, on the pipeline between the bidirectional electromagnetic valve D6 and the feed inlet of chromatographic column according to It is secondary that infusion pump P4, bidirectional electromagnetic valve D20, Unidirectional solenoid valve are installed；

A Unidirectional solenoid valve is connected at the feed inlet of the chromatographic column, Unidirectional solenoid valve is connect with bidirectional electromagnetic valve D20, two-way Solenoid valve D20 is connect with downcomer, and the discharge port of chromatographic column is divided into water outlet and eluent outlet, and water outlet connection water outlet is single To solenoid valve, eluent outlet connection water outlet bidirectional electromagnetic valve, the eluent outlet of chromatographic column is through water outlet bidirectional electromagnetic valve difference It is connect with High Purity horizontal tank and low purifying horizontal tank feed inlet, between the water outlet bidirectional electromagnetic valve and low purifying horizontal tank Bidirectional electromagnetic valve D25 is installed on pipeline；The water outlet of chromatographic column is through being discharged the feed inlet of Unidirectional solenoid valve and sewage treatment pot Connection；

The feed inlet of the sewage treatment pot is connect through Unidirectional solenoid valve S23 with running water pipe, and discharge port is through Unidirectional solenoid valve S24 It is connect with downcomer；

The feed inlet of the High Purity horizontal tank is connect through Unidirectional solenoid valve S22 with running water pipe, and discharge port is through bidirectional electromagnetic valve D12 is connect with downcomer and infusion pump P5 respectively, and infusion pump P5 is connect with bidirectional electromagnetic valve D3；

The feed inlet of the low purifying horizontal tank is connect through Unidirectional solenoid valve S37 with running water pipe, and discharge port is through bidirectional electromagnetic valve D13 is connect with downcomer and infusion pump P6 respectively, and infusion pump P6 is connect with bidirectional electromagnetic valve D3；

The feed inlet of the pure water tank is connect through Unidirectional solenoid valve S25 with running water pipe, discharge port through pipeline respectively with downcomer It is connected with the Unidirectional solenoid valve of chromatographic column, is sequentially installed with bi-directional electromagnetic on the pipeline between the discharge port and Unidirectional solenoid valve Valve D14, infusion pump P7, Unidirectional solenoid valve S20, downcomer are connect with bidirectional electromagnetic valve D14；

The feed inlet of the parsing tank is connect through Unidirectional solenoid valve S26 with running water pipe, and discharge port is distinguished through bidirectional electromagnetic valve D15 It is connect with infusion pump P7 and downcomer；

It is described acid tank feed inlet connect through Unidirectional solenoid valve S28 with running water pipe, discharge port through bidirectional electromagnetic valve D16 respectively with Infusion pump P7 is connected with downcomer；

The feed inlet of the alkali tank is connect through Unidirectional solenoid valve S30 with running water pipe, discharge port through bidirectional electromagnetic valve D17 respectively with Infusion pump P7 is connected with downcomer；

The discharge port of the blend tank is connect with infusion pump P8 and running water pipe respectively by bidirectional electromagnetic valve D18, infusion pump P8 It is connect respectively with the feed inlet of Unidirectional solenoid valve S1 and parsing tank, sour tank, alkali tank through bidirectional electromagnetic valve D24, the bi-directional electromagnetic Unidirectional solenoid valve S27, bidirectional electromagnetic valve D24 and sour tank feed inlet are installed on the pipeline between valve D24 and parsing tank feed inlet Between pipeline on Unidirectional solenoid valve S29 is installed, list is installed on the pipeline between bidirectional electromagnetic valve D24 and alkali tank feed inlet To solenoid valve S31；

The feed inlet of the solvent recovery tank is connect with running water pipe and recycling design pipe respectively through pipeline, and discharge port is through two-way electricity Magnet valve D22 is connect with downcomer and infusion pump P10 respectively, infusion pump P10 through pipeline respectively with blend tank and solvent tank into Material mouth connection, described, the pipeline connection between bidirectional electromagnetic valve D21 and infusion pump P8 and bidirectional electromagnetic valve D24, the infusion pump Bidirectional electromagnetic valve DK is installed on the pipeline between P10 and solvent tank；

The feed inlet of the solvent tank is connect through Unidirectional solenoid valve S33 with running water pipe, and discharge port is through bidirectional electromagnetic valve D19 points Pipeline not between downcomer, infusion pump P8 and bidirectional electromagnetic valve D18 is connect.

2. bioactive substance according to claim 1 isolates and purifies Process Control System, it is characterised in that the chromatography The quantity of column is 4~30.

3. bioactive substance according to claim 1 isolates and purifies the control method of Process Control System, feature exists In the method comprises the following steps:

One, extraction process:

Step 1: starting bidirectional electromagnetic valve D18 (0,2), infusion pump P8, bidirectional electromagnetic valve D24 (0,1) and Unidirectional solenoid valve S1, After solvent enters 100~120L in extraction kettle, bidirectional electromagnetic valve D18 (0,2), infusion pump P8, bidirectional electromagnetic valve D24 are closed (0,1) and Unidirectional solenoid valve S1；

Step 2: starting infusion pump P9, supersonic generator continuous extraction bioactive substance 30~60 minutes, close infusion Pump P9, supersonic generator；

Step 3: starting bidirectional electromagnetic valve D1 (0,2), infusion pump P1 and bidirectional electromagnetic valve DS5 (2,1) delay when extracting solution enters It rushes in tank after 100~120L, closes bidirectional electromagnetic valve D1 (0,2), infusion pump P1 and bidirectional electromagnetic valve DS5 (2,1)；

Step 4: step 1~3 1 time are repeated；

Two, concentration process:

Step 3: starting bidirectional electromagnetic valve D2 (0,2), infusion pump P2, bidirectional electromagnetic valve D3 (1,0), 100~120L extracting solution into After entering in inspissator, bidirectional electromagnetic valve D2 (0,2), infusion pump P2, bidirectional electromagnetic valve D3 (1,0) are closed, start inspissator, when mentioning When liquid being taken to be concentrated into 30~50L, inspissator is closed；

Step 4: opening three-way solenoid valve D4 (0,2), infusion pump P3, bidirectional electromagnetic valve D23 (0,1) and Unidirectional solenoid valve S13, After concentrate enters 30~40L in concentration storage tank, three-way solenoid valve D4 (0,2), infusion pump P3, bidirectional electromagnetic valve D23 are closed (0,1) and Unidirectional solenoid valve S13；

Step 5: open bidirectional electromagnetic valve D5 (0,1), infusion pump P3, bidirectional electromagnetic valve D23 (0,2), when enter solvent recovery tank In recycling design be 50~100L when, close bidirectional electromagnetic valve D5 (0,1), infusion pump P3, bidirectional electromagnetic valve D23 (0,2)；

Three, purification process:

Step 1: bidirectional electromagnetic valve D6 (0,2), infusion pump P4, bidirectional electromagnetic valve D20 (1,0) are opened；Unidirectional solenoid valve is opened, Each chromatography column volume that control concentrate enters chromatographic column is 8L, closes valve when reaching 8L, when entirely reaching 8L, is closed Bidirectional electromagnetic valve D6 (0,2), infusion pump P4, bidirectional electromagnetic valve D20 (1,0)；

Step 2: bidirectional electromagnetic valve D14 (0,2), infusion pump P7, Unidirectional solenoid valve S20, bidirectional electromagnetic valve D25 (0,2) are opened； Unidirectional solenoid valve is opened, is discharged bidirectional electromagnetic valve (0,2), is 64~96L by Unidirectional solenoid valve control pure water inlet, reaches Valve is closed when 64~96L, when inlet entirely reaches 64~96L, closes bidirectional electromagnetic valve D14 (0,2), bidirectional electromagnetic valve D25 (0,2), while flow, 10~32L/h of flow-control scope are controlled by water outlet bidirectional electromagnetic valve；

Step 3: when bidirectional electromagnetic valve D14 (0,2) close when, starting bidirectional electromagnetic valve D15 (0,2), bidirectional electromagnetic valve D25 (0, 1), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve, water outlet bidirectional electromagnetic valve (0,2) are in starting state at this time, by going out Water bidirectional electromagnetic valve controls flow and concentration conversion, flow-control scope: 10~32L/h, when any chromatography post detection is to highly concentrated When spending, bidirectional electromagnetic valve valve is discharged by (0,2) state and is converted to (0,1) state, while opening Unidirectional solenoid valve S21；When appoint One chromatographic column detects when becoming low concentration again from high concentration, is discharged bidirectional electromagnetic valve by (0,1) state and is converted to (0,2) shape State simultaneously closes off Unidirectional solenoid valve S21；

Step 4: when refined solution reaches 150~160L in High Purity horizontal tank, bidirectional electromagnetic valve D12 (0,2), infusion are opened P5, bidirectional electromagnetic valve D3 are pumped, into inspissator, when flow reaches 150~160L, is closed bidirectional electromagnetic valve D12 (0,2), defeated It is liquid pump P5, two-way to solenoid valve D5, prepare starting inspissator；

Step 5: according to concentration step one and two, starting inspissator, when high-purity eluent is concentrated into 15~30L, closes dense Contracting device starts three-way solenoid valve D4 (0,3), collects high-purity concentrate；

Step 6: open bidirectional electromagnetic valve D5 (0,1), infusion pump P3, bidirectional electromagnetic valve D23 (0,2), when recycling design all into When entering in solvent recovery tank, bidirectional electromagnetic valve D5 (0,1), infusion pump P3, bidirectional electromagnetic valve D23 (0,2) are closed；

Four, solvent recovery process:

Step 1: after High Purity liquid is concentrated, step four~six in purification process is repeated, low refined solution solvent recovery is carried out Prepare；

Step 2: low-purity chromatographic solution in low purifying horizontal tank is put into inspissator, starting bidirectional electromagnetic valve D13 (0,2), defeated Liquid pump P6, bidirectional electromagnetic valve D3 (0,1) are closed after the emptying of low purifying horizontal tank；The step of repeating two, concentration process one to Step 5 obtains low pure concentrate；It opens three-way solenoid valve D4 (0,1) to take out low pure concentrate, three-dimensional electromagnetism is closed after taking-up Valve D4；

Step 3: when recycling design is close to maximum volume in inspissator solvent recovery tank, starting bidirectional electromagnetic valve D5 (0,1), Infusion pump P3, bidirectional electromagnetic valve D23 (0,2) after emptying, close bidirectional electromagnetic valve D5 (0,1), infusion pump P3, bidirectional electromagnetic valve D23(0,2)；

Step 4: when recycling amount of alcohol reaches maximum volume in solvent recovery tank 4, starting bidirectional electromagnetic valve D22 (0,2) is stirred Mix pump P9, bidirectional electromagnetic valve Dk (0,2)；

Five, activation process:

Step 1: starting Unidirectional solenoid valve S19, Unidirectional solenoid valve, water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49, one hour Afterwards, Unidirectional solenoid valve S19, Unidirectional solenoid valve, water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49 are closed respectively；

Step 2: starting bidirectional electromagnetic valve D14 (0,2), infusion pump P7, Unidirectional solenoid valve S20, in chromatographic column inflow up to 16~ Bidirectional electromagnetic valve D14 (0,2), infusion pump P7, Unidirectional solenoid valve S20 are closed when 32L；After 6~8 hours, the unidirectional electricity of starting water outlet Magnet valve, Unidirectional solenoid valve S49 close water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49 after emptying；

Step 3: starting bidirectional electromagnetic valve D16 (0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve, into sewage When acid intake amount reaches 16~32L in process tank 17, chromatographic column, bidirectional electromagnetic valve D16 (0,2), infusion pump P7, unidirectional electromagnetism are closed Valve S20, Unidirectional solenoid valve；After 6~8 hours, starting water outlet Unidirectional solenoid valve closes water outlet Unidirectional solenoid valve after emptying；

Step 4: starting Unidirectional solenoid valve S19, Unidirectional solenoid valve, water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49, two hours Afterwards, Unidirectional solenoid valve S19 is closed respectively, and water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49 are closed after tap water emptying；

Step 5: starting bidirectional electromagnetic valve D17 (0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve, in chromatographic column When reaching 16~32L into alkali number, bidirectional electromagnetic valve D17 (0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve are closed； After 6~8 hours, starting water outlet Unidirectional solenoid valve closes water outlet Unidirectional solenoid valve after emptying into sewage treatment pot；

Step 6: starting Unidirectional solenoid valve S19, Unidirectional solenoid valve, water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49, two hours Afterwards, Unidirectional solenoid valve S19 is closed, water outlet Unidirectional solenoid valve, Unidirectional solenoid valve S49 are closed after tap water emptying；

Step 7: starting bidirectional electromagnetic valve D15 (0,2), infusion pump P7, Unidirectional solenoid valve S20, Unidirectional solenoid valve, in chromatographic column When solvent input reaches 16~32L, bidirectional electromagnetic valve D15 (0,2), infusion pump P7, Unidirectional solenoid valve S20, unidirectional electromagnetism are closed Valve, it is stand-by；Next time is put into low purifying horizontal tank before purification, by solvent, opens water outlet bidirectional electromagnetic valve (0,2), two-way electricity Magnet valve D25 (0,1)；

Six, allocation process:

1, desorbed solution is deployed: starting bidirectional electromagnetic valve D19 (0,2), infusion pump P8, bidirectional electromagnetic valve D21 (1,2), inlet 50 ~200L starts bidirectional electromagnetic valve D22 (0,2), mixing pump P9, bidirectional electromagnetic valve D21 (0,2), 50~200L of inlet, starting Unidirectional solenoid valve S32,50~200L of inlet, starting stirring 30 minutes；

4, pure water: starting Unidirectional solenoid valve S25, inlet 300L；

Seven, cleaning process:

1, extraction kettle: starting Unidirectional solenoid valve S1 after reaching maximum volume, is closed；After impregnating 12 hours, start bidirectional electromagnetic valve D1 (0,1) is closed all after emptying；It is again started up Unidirectional solenoid valve S1, after reaching maximum volume, Unidirectional solenoid valve S1 is closed, opens It opens bidirectional electromagnetic valve D1 (0,1), all after emptying, closes, cleaning terminates；

2, extraction kettle, heater, heater hot water storage tank, surge tank, solvent recovery tank, inspissator, inspissator solvent recovery tank, Concentration storage tank, chromatographic column, High Purity horizontal tank, pure water tank, parsing tank, sour tank, alkali tank, blend tank, solvent tank, low purifying are sleeping Formula tank, sewage treatment pot press extraction kettle cleaning method.

4. control method according to claim 3, it is characterised in that the bioactive substance is polyphenol, flavones, pattern Glycosides, procyanidine, saponin, alkaloid, polysaccharide, amino acid, polypeptide or pigment.

5. control method according to claim 3, it is characterised in that in the extraction process, it is total that extractant accounts for extraction kettle The 1/2~3/4 of volume, solid-liquid ratio are 1:5~20, and the combining extraction liquid once and twice extracted accounts for the 1/2 of surge tank total volume ~3/4.

6. control method according to claim 3, it is characterised in that in the concentration process, extracting liquid volume accounts for inspissator The 1/4~1/2 of total volume is concentrated to the 1/3~1/5 of original volume.

7. control method according to claim 3, it is characterised in that in the purification process, the volume of the concentrated liquid accounts for chromatographic column The 1/4~1/5 of column volume, pure water consumption are 2~4 column volumes, and eluent dosage is 2~4 column volumes, and elution flow rate is 0.1~1 column volume/h, chromatographic column quantity are 4~30.

8. control method according to claim 3, it is characterised in that in the activation process, acid solution dosage is 1.5~1 A column volume, aqueous slkali dosage are 1.5~1 column volumes.

9. control method according to claim 3, it is characterised in that in the allocation process, the volumetric concentration 40 of desorbed solution ~80%, the mass-volume concentration of acid solution is 1~5%, and the mass-volume concentration of aqueous slkali is 1~5%.

10. control method according to claim 3, it is characterised in that water cleaning equipment 2 times, right in the cleaning process The cleaning of equipment can carry out simultaneously.