CN109776467A - A kind of gibberellic acid extracting method being concentrated using MVR technique - Google Patents
A kind of gibberellic acid extracting method being concentrated using MVR technique Download PDFInfo
- Publication number
- CN109776467A CN109776467A CN201811596456.3A CN201811596456A CN109776467A CN 109776467 A CN109776467 A CN 109776467A CN 201811596456 A CN201811596456 A CN 201811596456A CN 109776467 A CN109776467 A CN 109776467A
- Authority
- CN
- China
- Prior art keywords
- gibberellic acid
- concentrated
- mvr
- extracting method
- heater
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of gibberellic acid extracting methods being concentrated using MVR technique, comprising: the fermentation of step 1) gibberellic acid strain；Filtering fermentation liquor in step 1 is respectively obtained filtrate and filter residue by step 2)；Filtrate in step 2 is concentrated step 3) by MVR technique, obtains concentrate；Step 4) extracts the concentrate in step 3 using ethyl ester, separates ethyl ester afterwards, obtains gibberellic acid crude product；Step 5) post-processes the crude product in step 4, obtains gibberellic acid finished product.The present invention extracts in gibberellic acid and applies MVR in concentration process, is at home and abroad the first, its significance lies in that promoting the development of gibberellic acid technique, with the product feedback of high quality of products, low price in agriculture, is conducive to improve farmers' income, promotes growth of agricultural efficiency, increasing peasant income.
Description
Technical field
The present invention relates to biofermentations to extract field, mentions specifically, being related to a kind of gibberellic acid being concentrated using MVR technique
Take method.
Background technique
China is that appliable plant growth substance is most widely national in the world, and large-area applications plant is raw in agricultural production
Long regulator has made remarkable achievements, and continually develops utilization and chemical pesticide tune with plant growth regulator
The continuous development of control technology, gibberellic acid series of products are because its physiological activity is high, residual is less, safety is good and dosage form is more advanced
The advantages that, will more it be widely used in each link of agricultural production.
For the competitiveness for improving gibberellic acid market, energy-efficient condensing mode is selected, reduces energy consumption, effective save is produced into
This.How to solve former gibberellic acid to extract in film concentration process, energy utilization rate is low, distillation time is long, the big, people using quantity of steam
The disadvantages of member's operation is relatively complicated, becomes problem anxious to be resolved.
Summary of the invention
The technical problem to be solved by the present invention is in view of the deficiencies of the prior art, provide a kind of to be concentrated using MVR technique
Gibberellic acid extracting method.
The technical scheme to solve the above technical problems is that
The present invention provides a kind of gibberellic acid extracting method being concentrated using MVR technique, comprising:
The fermentation of step 1) gibberellic acid strain；
Filtering fermentation liquor in step 1 is respectively obtained filtrate and filter residue by step 2)；
Filtrate in step 2 is concentrated step 3) by MVR technique, obtains concentrate；
Step 4) extracts the concentrate in step 3 using ethyl ester, separates ethyl ester after taking methacrylate layer, it is thick to obtain gibberellic acid
Product；
Step 5) post-processes the crude product in step 4, obtains gibberellic acid finished product.
The beneficial effects of the present invention are: gibberellic acid, which extracts, applies MVR in concentration process, and it is at home and abroad the first, meaning
It is to promote the development of gibberellic acid technique, with the product feedback of high quality of products, low price in agriculture, is conducive to improve peasant's receipts
Enter, promotes growth of agricultural efficiency, increasing peasant income.Concentration uses MVR technique (steam mechanical recompression) distilling material, when distillation
Between shorten 3 more than hour, while shortening residence time of material, avoid the destruction of product, save 150 tons of steam or so daily,
45000 tons of steam or so will be saved every year, be produced a profit about 5,000,000 yuan.
Further, it in the step 3, is concentrated using MVR evaporation circulating system.
Further, the MVR evaporation circulating system includes preheater, heater, separator, compressor and circulating pump, object
Material heat temperature raising in the tubulation of preheater, is entered after heater feeding chamber by the bottom of heater be transported to heater later
Top feed and under the action of liquid distributor, uniformly enters in heating tube, quick flowing and gravity itself by steam
Effect material is flowed downward naturally along inside pipe wall in membranaceous, and it is heated be constantly concentrated by evaporation, reach after concentrate requirement through a left side plus
Bin bottom is delivered in fluid reservoir, obtains concentrate.The secondary low-grade steam generated during material evaporation, by vapour-liquid
It is transported to compressor after separator isolation of purified, is transported to heater after being promoted to high-grade steam heat source, is followed as MVR evaporation
The heating steam of loop system so recycles to vapo(u)rization system and provides thermal energy, realizes heat circulation continuous evaporation, to reduce external
The demand of boundary's energy.
Further, plate-frame filtering is filtered into the step 2.
Further, the separation method of ethyl ester is to be evaporated in vacuo partition method in the step 4.
Further, the post-processing in the step 5 includes the crystallisation by cooling, suction filtration and drying to gibberellic acid crude product.
Further, further include step 6, the gibberellic acid finished product in step 5 is detected, after detection is qualified, be packed and stored.
Detailed description of the invention
Fig. 1 is the gibberellic acid extracting method process flow chart of the invention being concentrated using MVR technique；
Fig. 2 is MVR evaporation circulating system process flow chart of the invention.
Drawing reference numeral explanation:
1. preheater, 2.MVR heater, 3.MVR vapour liquid separator, 4.MVR compressor, 5. concentrate receiving tanks.
Specific embodiment
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
As shown in Figure 1, the present invention provides a kind of gibberellic acid extracting method being concentrated using MVR technique, comprising: step 1) is red
The fermentation of mould acid strain；Filtering fermentation liquor in step 1 is respectively obtained filtrate and filter residue by step 2)；Step 3) will be in step 2
Filtrate be concentrated by MVR technique, obtain concentrate；Step 4) extracts the concentrate in step 3 using ethyl ester, takes second
Ethyl ester is separated after ester layer, obtains gibberellic acid crude product；Step 5) post-processes the crude product in step 4, obtains gibberellic acid finished product.
Wherein, it in the step 3, is concentrated using MVR evaporation circulating system.As shown in Fig. 2, the MVR evaporation follows
Loop system includes preheater 1, heater 2, separator 3, compressor 4 and circulating pump, the flow channel for liquids import of the preheater 1 with
The hot condensed water outlet of the collet of heater 2 is connected, and the flow channel for liquids outlet of the preheater 1 is connected with cooling water pipeline
Logical, the material inlet of the preheater 1 receives filtrate, the charging of the feeding chamber of the material outlet and heater 2 of the preheater 1
Portion's (i.e. right part of figure upper heater lower part) is connected；Discharging portion (the i.e. figure upper heater of the feeding chamber of the heater 2
The left part of lower part) it is connected with concentrate receiving tank；It is connected between the feeder and discharging portion by heating tube, is added
It is the material of flowing in heat pipe, is heated on the outside of heating tube by the steam of collet；The top of heating tube is arranged in liquid distributor,
Heating tube is equipped with the steam (vapor) outlet being connected with separator, and the steam is by realizing gas-liquid separation with separator 3, after separation
Gas by compressor 4 compress after be transported to collet or steam pipework, liquid reflux is into heating tube after separation.Material exists
The hot condensed water heat temperature raising being discharged in the tubulation of preheater 1 by 2 collet of heater, later under the action of circulating pump material by
Bottom enters the feeding chamber of heater 2, and the material in feeding chamber is transported to the top feed of heater 2 by circulating pump, is adding
Material in hot device 2 uniformly enters in heating tube under the action of liquid distributor, quick flowing and weight itself by steam
Power acts on material and is flowed downward naturally along inside pipe wall in membranaceous, and it is heated be constantly concentrated by evaporation, reach after concentrate requirement through a left side
Feeding chamber bottom is delivered to subsequent processing.The secondary low-grade steam generated during material evaporation, by vapour liquid separator 3
It is transported to compressor 4 after isolation of purified, is transported to heater 2 after being promoted to high-grade steam heat source, as MVR vaporization cycle system
The heating steam of system so recycles to vapo(u)rization system and provides thermal energy, realizes heat circulation continuous evaporation, to reduce to extraneous energy
The demand in source.Plate-frame filtering is filtered into the step 2.The separation method of ethyl ester is to be evaporated in vacuo separation in the step 4
Method.Post-processing in the step 5 includes the crystallisation by cooling, suction filtration and drying to gibberellic acid crude product.It further include step 6, to step
Gibberellic acid finished product in rapid 5 is detected, and after detection is qualified, is packed and stored.
Embodiment 1
96 tons of gibberellin fermented liquid of the fermented culture of gibberellin strain, 2200 μ of potency/ml are taken, fermentating liquid PH value is
3.6, add the sour 50kg of content 40%, pH value is adjusted to 2.0；Filtrate is extruded through plate compression device；Filtrate is followed using MVR evaporation
Loop system is concentrated, and thickening temperature is 48-52 DEG C, and 4 hours are concentrated, and the pH value of concentrate is 2.0-2.5 after concentration；This
About 80% moisture is fallen in concentration by concentration process；As shown in Fig. 2, in MVR concentration process of the invention, after plate-frame filtering
Filtrate is sent after first passing through the preheating of preheater into MVR heater 2, is transported to MVR heater top feed by circulating pump,
Feed liquid enters in heating tube through distributor by thermal evaporation in MVR heater 2.Liquid and secondary low-grade steaming in evaporation process
Vapour enters vapour liquid separator 3, carries out vapor-liquid separation in vapour liquid separator 3, the liquid after separation, which returns in MVR heater 2, to be continued
Concentration, the low-grade steam after separation are transported to compressor 4, and compressor 4 is steamed high-grade is promoted to after low-grade both vapor compression
Vapour is transported in MVR heater, as the heating steam of MVR evaporation circulating system, is so recycled to vapo(u)rization system and is provided thermal energy,
Heat circulation continuous evaporation is realized, to reduce the demand to outside resources.The concentrate being finally concentrated passes through MVR heater
The left feed bin in 2 bottoms is conveyed and is stored in concentrate receiving tank.
Ethyl ester is added according to the volume ratio of 1:1.1 in concentrate to be extracted, 10-15 clock is stirred, makes red mould sufficiently molten
Solution is separated in ethyl ester solvent by liquid-liquid-solid disc centrifuge, since water is different from the specific gravity of ethyl ester, the specific gravity of water
It is higher more first to throw out, it throws out after the specific gravity of ethyl ester relatively light time, therefore, it is recycled respectively.Through obtained by extraction and separation
Ethyl ester light liquid, be conveyed to single pot of distillation, using 0.5-1kg negative pressure, the ethyl ester in ethyl ester light liquid be at high temperature steam evaporation,
And the ethyl ester evaporated recycling is used for next batch and is produced, the gibberellic acid feed liquid in ethyl ester light liquid is concentrated in single pot of distillation, passes through
Crystallisation by cooling obtains gibberellic acid crude product 183kg after suction filtration；
Ethyl ester, the dissolution of alcohol mixed solvent of 1:1.5 are added in gibberellic acid crude product, is conveyed to single pot of distillation, uses
0.5-1kg negative pressure, ethyl ester, alcohol are miscible to be evaporated in steam at high temperature, and the miscible recycling evaporated is used for next batch
It produces, is filtered to obtain gibberellic acid crystal powder within gibberellic acid feed liquid crystallisation by cooling 3 hours or more in single pot, by baking oven 70
It was dried at DEG C through 10-12 hours, obtains 93.2% gibberellic acid finished product 152kg.
Using MVR technique, i.e. steam mechanical recompression, it is exactly the secondary steam generated using evaporation, passes through machinery
Secondary low-grade steam is compressed in compression, converts high-grade steam for its saturation temperature raising 8-11 degree, as
Heat source introduces heater and heats room, carries out heating vaporization to material, makes entirely to evaporate in addition to the electric energy that compressor consumes, substantially not
Steam is consumed, and the electric energy of the water pump of power consumption and original system, hydraulic ejector water pump remains basically stable, and equipment can be large-scale
Change, automation.This technique is used for the extraction of gibberellic acid product, thoroughly solves energy utilization rate in former extraction film concentration process
It is low, distillation time is long, using quantity of steam, big, personnel operate the disadvantages of relatively complicated.MVR technique can shorten residence time of material,
Avoiding the destruction of product structure, whole year saves about 45000 tons of steam, reduce 5787 tons of coal of mark, about 5,000,000 yuan of Nian Zengjia profit,
And concentration post no longer generates sewage, condensed water is purer, can directly return production system use.
A kind of gibberellic acid extracting method being concentrated using MVR technique of the invention uses energy-efficient condensing mode, as far as possible
Reduction be concentrated energy consumption.The low-grade steam separated from separator, by compressor compresses, pressure and temperature is increased, heat
Enthalpy increases, and the heating room for then arriving heater is used as heating steam, so that feed liquid is maintained fluidized state, originally to discard in this way
Steam be fully utilized, recycled latent heat, improved efficiency of heating- utilization；
Meanwhile using continuous production, labor productivity, lower cost of wheeling are improved.Raw steam is utilized by heater
After primary, the most low-grade energy contained in the steam of generation collects by compressor and is spending very little electricity
On the basis of the cost of energy, this some vapor is risen into the high-quality energy, heater is sent back to and is used as heat source.Continuous production contracting
The short distillation residence time, the destruction to product is avoided, 150 tons of steam can be saved daily；
A kind of gibberellic acid extracting method being concentrated using MVR technique of the invention uses energy-efficient condensing mode, using PLC
The automatic operating of control, high degree of automation, operating cost is low, easy to operate, there is significant source benefit and environmental benefit.
Application of the MVR technology in gibberellic acid extraction process is an energy saving approach.Utilize the secondary pressure of steam
It is condensed to evaporation and heat is provided, saved a large amount of steam.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of gibberellic acid extracting method being concentrated using MVR technique characterized by comprising
The fermentation of step 1) gibberellic acid strain；
Filtering fermentation liquor in step 1 is respectively obtained filtrate and filter residue by step 2)；
Filtrate in step 2 is concentrated step 3) by MVR technique, obtains concentrate；
Step 4) extracts the concentrate in step 3 using ethyl ester, separates ethyl ester after taking methacrylate layer, obtains gibberellic acid crude product；
Step 5) post-processes the crude product in step 4, obtains gibberellic acid finished product.
2. a kind of gibberellic acid extracting method being concentrated using MVR technique according to claim 1, which is characterized in that described
In step 3, it is concentrated using MVR evaporation circulating system.
3. a kind of gibberellic acid extracting method being concentrated using MVR technique according to claim 2, which is characterized in that described
MVR evaporation circulating system includes preheater, heater, separator, compressor and circulating pump, and material adds in the tubulation of preheater
Heat heating is entered after heater feeding chamber by the bottom of heater later and is transported to heater top feed and is distributed in feed liquid
It under the action of device, uniformly enters in heating tube, the quick flowing and gravity material itself by steam are in film along inside pipe wall
Shape flows downward naturally, and it is heated be constantly concentrated by evaporation, reach and be delivered to fluid reservoir through left feeding chamber bottom after concentrate requirement
In, obtain concentrate.
4. a kind of gibberellic acid extracting method being concentrated using MVR technique according to claim 1, which is characterized in that described
Plate-frame filtering is filtered into step 2.
5. a kind of gibberellic acid extracting method being concentrated using MVR technique according to claim 1, which is characterized in that described
The separation method of ethyl ester is to be evaporated in vacuo partition method in step 4.
6. a kind of gibberellic acid extracting method being concentrated using MVR technique according to claim 1, which is characterized in that described
Post-processing in step 5 includes the crystallisation by cooling, suction filtration and drying to gibberellic acid crude product.
7. a kind of -6 any gibberellic acid extracting method being concentrated using MVR technique, feature are existed according to claim 1
In further including step 6, detected to the gibberellic acid finished product in step 5, after detection is qualified, is packed and stored.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811596456.3A CN109776467B (en) | 2018-12-26 | 2018-12-26 | Gibberellic acid extraction method using MVR (mechanical vapor recompression) process for concentration |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811596456.3A CN109776467B (en) | 2018-12-26 | 2018-12-26 | Gibberellic acid extraction method using MVR (mechanical vapor recompression) process for concentration |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109776467A true CN109776467A (en) | 2019-05-21 |
| CN109776467B CN109776467B (en) | 2023-02-21 |
Family
ID=66498353
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811596456.3A Active CN109776467B (en) | 2018-12-26 | 2018-12-26 | Gibberellic acid extraction method using MVR (mechanical vapor recompression) process for concentration |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109776467B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134751A (en) * | 2007-03-12 | 2008-03-05 | 江苏丰源生物化工有限公司 | Method for extracting gibberellic acid GA4+7 from gibberellic acid fermentation liquor |
| US20080085543A1 (en) * | 2006-09-15 | 2008-04-10 | Reliance Life Sciences Pvt. Ltd. | Process for gibberellic acid production with "fusarium moniliforme" strains |
| CN104524807A (en) * | 2015-01-25 | 2015-04-22 | 陈式好 | MVR (Mechanical Vapor Recompression) continuous evaporating crystallizing system |
-
2018
- 2018-12-26 CN CN201811596456.3A patent/CN109776467B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080085543A1 (en) * | 2006-09-15 | 2008-04-10 | Reliance Life Sciences Pvt. Ltd. | Process for gibberellic acid production with "fusarium moniliforme" strains |
| CN101134751A (en) * | 2007-03-12 | 2008-03-05 | 江苏丰源生物化工有限公司 | Method for extracting gibberellic acid GA4+7 from gibberellic acid fermentation liquor |
| CN104524807A (en) * | 2015-01-25 | 2015-04-22 | 陈式好 | MVR (Mechanical Vapor Recompression) continuous evaporating crystallizing system |
Non-Patent Citations (1)
| Title |
|---|
| 高丽丽等: "MVR蒸发与多效蒸发技术的能效对比分析研究", 《现代化工》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109776467B (en) | 2023-02-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102286544B (en) | A kind of clean preparation method of starch base alcohol fuel | |
| CN104787823B (en) | Yeast wastewater Zero discharge treatment method | |
| CN104151136B (en) | The processing method of butanols-N-BUTYL ACETATE is reclaimed from antibiotic production wastewater | |
| CN101445449A (en) | Production method and device for sodium gluconate energy-saving triple effect concentration and crystallization | |
| CN104926675A (en) | Recovery process of low concentration dimethylacetamide | |
| CN103394205B (en) | Molasses alcohol fermented mature mash multi-effect evaporation concentration integrated equipment and process | |
| CN206304378U (en) | The energy-conservation MVR evaporators that a kind of vapor recompression is utilized | |
| CN207871571U (en) | A kind of evaporating, concentrating and crystallizing system | |
| CN101735012B (en) | Method for separating and extracting 2,3-butanediol | |
| CN204815733U (en) | Distillation preheating device | |
| CN207980445U (en) | Alcohol extracting liquid evaporates and ethyl alcohol rectification coupling apparatus | |
| CN109776467A (en) | A kind of gibberellic acid extracting method being concentrated using MVR technique | |
| CN107827778B (en) | Device and process for refining cyanoacetic acid ester by continuous rectification | |
| CN207904089U (en) | Pickles high-salt wastewater MVR desalination biochemical devices | |
| CN205313431U (en) | Cyanoacetic acid ester and malonate's continuous cyaniding separator | |
| CN205235415U (en) | Thermal cycle mechanical compression evaporation plant | |
| CN212769939U (en) | Treatment system for cellulose production wastewater | |
| CN212491600U (en) | Novel stirring dewatering device of proline automatic control temperature | |
| CN210813975U (en) | Double ethyl methyl ester efficient energy-saving distillation device | |
| CN210096970U (en) | Furfural multiple-effect reaction rectifying device | |
| CN101391782B (en) | Method for simultaneously producing two different content industry anhydrous sodium sulfate | |
| CN207537373U (en) | A kind of continuous rectification refines cyanoacetate compound device | |
| CN112494536A (en) | Preparation method of medicine extract for treating nasal diseases | |
| CN102442884B (en) | Method for recovering ethanol during soy production process and device thereof | |
| CN202173793U (en) | Alcohol prefractionator reboiling system using centrifugal clear liquid as cyclic medium |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |