CN1118775A - Method for producing solanesol - Google Patents
Method for producing solanesol Download PDFInfo
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- CN1118775A CN1118775A CN 94115570 CN94115570A CN1118775A CN 1118775 A CN1118775 A CN 1118775A CN 94115570 CN94115570 CN 94115570 CN 94115570 A CN94115570 A CN 94115570A CN 1118775 A CN1118775 A CN 1118775A
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- buddhist nun
- solvent
- eggplant buddhist
- nun alcohol
- production method
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Based on the existing technology for producing solanesol, the present method changes the process of intermittent extraction into continuous one, and adds twice settling process and tail-gas absorption process. Advantage low solvent oil consumption, less environment pollution and high product quality.
Description
The present invention relates to a kind of production method of eggplant Buddhist nun alcohol.
Eggplant Buddhist nun alcohol is a kind of pharmaceutical purpose material, and it can be used as medical auxilliary mould Q
10(controlling heart disease) and vitamin K
2Side switch, itself also promises to be the material of medical effect.Publication number CN1056486A patent specification discloses the method for preparing eggplant Buddhist nun alcohol with mould cigarette or broken offal, its industrial normal hexane or No. 6 solvent oils with 60-80% carry out extracting as extraction solvent, after handling, multistep obtains product, because this method exists following defective, therefore cause solvent-oil ratio big, the product cost height, qualification rate is low, topsoil is serious, can't form the suitability for industrialized production scale.Its defective is as follows: one, adopts twice and is interrupted extraction process, and total system shortage tail gas recycle process, make volatile extraction solvent evaporate in a large number in the air, not only contaminate environment endangers safety, and has wasted a large amount of extraction solvents, the product cost height.Two, make extractor with reactor raw material is carried out the extracting of twice interruption, mechanization degree is low, the production cycle is long, yields poorly, and can't form scale and benefit.Three depend merely on gained mixing oil after the filtration, purification extracting, are difficult to guarantee the key technical indexes-" flowability of acetone insoluble matter " qualified of eggplant Buddhist nun alcohol product.
The purpose of this invention is to provide a kind of waste that can reduce extraction solvent, reduce product cost, guarantee quality product, and be suitable for the production method of the eggplant Buddhist nun alcohol of large-scale industrial production.
The object of the present invention is achieved like this:
A kind of production method of eggplant Buddhist nun alcohol, it is characterized in that: it may further comprise the steps,
(1) raw material crushing, oven dry pre-treatment;
(2) pretreated raw material carries out continuous extracting with solvent for extraction in flat rotary extractor, draws the mixing oil and the scarp that contain eggplant Buddhist nun alcohol;
(3) carry out a sedimentation behind the hybrid oil filter, carry out normal pressure then and concentrate;
(4) mixing oil after concentrating carries out getting product through concentrating under reduced pressure again behind the secondary settlement;
(5) step (2) gained scarp adopts the method for open steam heating, indirect steam oven dry to reclaim solvent oil;
(6) tail gas recycle in the above steps.
Described solvent for extraction can be industrial normal hexane or 6
#Solvent oil, described raw material in flat rotary extractor through continuous 5 hydro-peening extractings of two hours.
The described once settled time is 30-40 minute, and mixing oil enters after 180-240 order filter cloth filters and rises membrane type long-tube evaportor normal pressure and concentrate after the sedimentation, and its vaporization temperature is 75-85 ℃.
The time of described secondary settlement is 1.8-2.5 hour, and the vacuum tightness of concentrating under reduced pressure is 0.07-0.08MPa thereafter, and insulation was 2-3 hour when liquidus temperature was 80-85 ℃.
Described scarp solvent recuperation selects for use high bed of material steaming-drying machine to carry out, and the open steam pressure of feeding is 0.07-0.1MPa, and the pressure of indirect steam is 0.5-0.8MPa
Tail gas reclaims with vegetables oil in the absorption tower in the above steps, and described absorption tower non-condensable gas outlet pipe is connected with vacuum pump, and the vacuum tightness that makes exhaust system is 0.001-0.003MPa.
Fig. 1 is a process flow sheet of the present invention
The present invention is owing to adopt aforementioned production method, the prerequisite that not only can ensure the quality of products The large-scale industrial production of lower realization high yield, and can save a large amount of solvent for extraction, Reduced product cost.
At first, replace publication number CN10 with flat rotary extractor as extractor Reactor in the 56486A patent application is so that publication number CN10564 Be interrupted extractive process and change 5 in the flat rotary extractor into for twice in the 86A patent application Inferior continuous extracting has been saved the working time greatly, has improved output, can satisfy industry Change requirement.
The second, increase by two step infall processes. For the first time sedimentation is in order tentatively to remove impurity Prevent the obstruction of screen pack, the purpose of for the second time sedimentation be for further remove silt, The impurity such as scarp, thereby the quality of assurance product. The sedimentation time second time and product below The product the ash content of coal test result table of comparisons:
| Time | Ash % |
| 1.5 | 1.0 |
| 1.8 | 0.8 |
| 2.0 | 0.5 |
| 2.5 | 0.1 |
As can be seen from the above table, the sedimentation time is 1.8 hours for the second time, the ash content of coal Can meet quality standard≤0.8%, and the content of ash directly has influence on product The flowability of the key technical indexes acetone insoluble matter ".
This twice sedimentation avoided in the publication number CN1056486A patent application, Do not conform to owing to only removing the product that the impurity such as scarp and silt causes in the product by filtration Lattice have guaranteed the quality of product. The present invention and CN1056486A below The up-to-standard rate table of comparisons of disclosed technical products in the patent application:
Annotate: every crowd of 825Kg
| Project | Output | Certified products | Defective work | Qualification rate |
| CN105648A | 5 batches | 3 batches | 2 batches | 60％ |
| The present invention | 20 batches | 20 batches | 0 batch | 100％ |
Three, adopt the absorption tower that the solvent for extraction in the tail gas in each step is carried out plant Oil absorbs, and has not only reclaimed a large amount of extraction solvents, has also reduced pollution and safety hazard. Simultaneously, adopt little negative pressure technique of exhaust system, make whole system be in micro-vacuum state, Reduce the generation of run, drip, leak phenomenons, more met industrial requirement. The party Method is produced Salanesol product per ton need only 2 tons of solvent for extraction, compare CN10564 Disclosed technology is produced Salanesol product per ton and can be saved 6 tons in the 86A patent application Solvent for extraction reduces cost more than 15000 yuan.
Four, adopt the high bed of material dryer scarp to be heated indirect steam with live (open) steam The method of oven dry is processed, simple than in the CN1056486A patent application With the solvent for extraction in the method recovery scarp of indirect steam oven dry, meeting in assurance will Can save a large amount of time in the situation about asking. The present invention and CN10564 below The used time table of comparisons of scarp is processed in the 86A patent application
Annotate: the time is that the scarp processing meets standard (containing solvent naphtha≤0.15%) in the upper table The used time.
| CN1056486A | The present invention | |
| Time | 3h | 1.5h |
In addition, this process adopts flat rotary extractor, film-rising evaporator, high material After the higher a whole set of extractings of equipment composition of mechanization degree such as layer dryer, settling tank reach Treatment system makes the method realize heavy industrialization, and personnel, energy consumption reduce, produce Amount improves. Integrated cost has descended 50%. The present invention and CN1056 below The disclosed technology Expenditure Levels of the 486A patent application table of comparisons:
| The project technology category | The personnel directly engaged in production | Solvent consumption (t) | During power consumption kw/ | During water consumption t/ | During consumption steam t/ | Daily production capacity kg |
| CN1056486A | 40 | 8 tons | 30 | 20 | 0.3 | 70 |
| The present invention | 40 | 2 tons | 40 | 20 | 0.7 | 400 |
| CN1056486A is multiple of the present invention | 5.7 doubly | 4 times | 4.2 doubly | 5.7 doubly | 2.4 doubly | After being equivalent to improve 17% |
The present invention is described in detail below in conjunction with embodiment.
A kind of production method of eggplant Buddhist nun alcohol, it may further comprise the steps:
1, chooses mould cigarette or the broken offal that contains eggplant Buddhist nun alcohol 〉=1%, dry behind the removal offal, make its water content≤2.1%.
2, pretreated raw material is sent in the flat rotary extractor with scraper conveyor, and inlet amount is every two hours 1080 kilograms, simultaneously with 18M per hour
3Flow in leacher, carry 6
#Solvent oil.The raw material cigarette obtains containing the mixing oil and the scarp of eggplant Buddhist nun alcohol through 5 hydro-peening extractings of two hours in leacher.
3, mixing oil at first enters the slurry tank quiescent settling one time after coarse filtration, and sedimentation this time is preliminary sedimentation, its objective is that its settling time is 35 minutes in order to prevent the obstruction of postorder filtration procedure filter screen.Enter after mixing oil after the sedimentation filters with 200 purpose silk screens or non-woven fabrics and rise the membrane type long-tube evaportor and carry out atmospheric evaporation and concentrate, evaporator temperature is controlled to be 80 ℃, liquid after the evaporation is concentrated blend, and gaseous solvent enters the solvent cycle cabinet and participates in circulation after condensation.
4, concentrated blend enters the secondary settlement jar, is evacuated to the concentrating under reduced pressure still and carries out concentrating under reduced pressure behind 2 hours secondary settlement, and its vacuum degree control is at 0.075MPa, and liquidus temperature is 83 ℃, heat-insulation pressure keeping 2.5 hours, get final product product.
5, the gained scarp is delivered in the high bed of material steaming-drying machine of preheating with scraper conveyor in the step 2, carry out twice heating recovery solvent of open steam and indirect steam, high bed of material steaming-drying machine upper strata open steam pressure is 0.08MPa, lower floor's indirect steam pressure is 0.07MPa, recovered solvent enters the solvent cycle cabinet through condensation, after dividing water and participates in circulation, and scarp drops down onto through the automatic blanking door slags tap auger and export.
6, the tail gas in above-mentioned each process is behind the tail gas surge tank, enter condenser condenses, do not coagulate solvent gas and enter the absorption tower, absorb with vegetables oil, absorption tower non-condensable gas outlet pipe is connected with water-jet pump, make total system all be in the micro-vacuum state that vacuum tightness is 0.002MPa, reduced the generation of total system run, drip, leak phenomenons.
The quality of the product that makes with aforesaid method is:
Weight loss on drying≤3%, standard is :≤6%.
Eggplant Buddhist nun alcohol content 〉=20%, standard is: 〉=16.5%.
The flowability of acetone insoluble matter: A, standard is: A subtract be qualified.
Wherein: the flowability of acetone insoluble matter, specify Tianjin department of chemistry of Nankai University of detection unit to detect by this index.Weight loss on drying, eggplant Buddhist nun alcohol content's index are detected by Tianjin inspection center of Nankai University.
Get eggplant Buddhist nun alcohol per ton with aforesaid method and need to consume 2 tons of solvents.
Claims (6)
1, a kind of production method of eggplant Buddhist nun alcohol, it is characterized in that: it may further comprise the steps,
(1) raw material crushing, oven dry pre-treatment;
(2) pretreated raw material carries out continuous extracting with solvent for extraction in flat rotary extractor, draws the mixing oil and the scarp that contain eggplant Buddhist nun alcohol;
(3) carry out a sedimentation behind the hybrid oil filter, carry out normal pressure then and concentrate;
(4) mixing oil after concentrating carries out carrying out concentrating under reduced pressure behind the secondary settlement and gets product;
(5) step (2) gained scarp adopts the method for open steam heating, indirect steam oven dry to reclaim solvent;
(6) tail gas recycle in the above steps.
2, the production method of a kind of eggplant Buddhist nun alcohol as claimed in claim 1 is characterized in that: described solvent for extraction is industrial normal hexane or 6
#Solvent oil, described raw material in flat rotary extractor through continuous 5 hydro-peening extractings of two hours.
3, the production method of a kind of eggplant Buddhist nun alcohol as claimed in claim 1, it is characterized in that: the described once settled time is 30-40 minute, mixing oil enters after 180-240 order filter cloth filters and rises membrane type long-tube evaportor normal pressure and concentrate after the sedimentation, and its vaporization temperature is 75-85 ℃.
4, the production method of a kind of eggplant Buddhist nun alcohol as claimed in claim 1 is characterized in that: the time of described secondary settlement is 1.8-2.5 hour, and the vacuum tightness of concentrating under reduced pressure is 0.07-0.08MPa thereafter, and insulation was 2-3 hour when liquidus temperature was 80-85 ℃.
5, the production method of a kind of eggplant Buddhist nun alcohol as claimed in claim 1 is characterized in that: described scarp reclaims solvent and selects for use high bed of material dryer to carry out, and the open steam pressure of feeding is 0.07-0.1MPa, and the pressure of indirect steam is 0.5-0.8MPa.
6, the production method of a kind of eggplant Buddhist nun alcohol as claimed in claim 1, it is characterized in that: tail gas reclaims with vegetables oil in the absorption tower in each step, and described absorption tower non-condensable gas outlet pipe is connected with vacuum pump, and the vacuum tightness that makes exhaust system is 0.001-0.003MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94115570 CN1118775A (en) | 1994-09-15 | 1994-09-15 | Method for producing solanesol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94115570 CN1118775A (en) | 1994-09-15 | 1994-09-15 | Method for producing solanesol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1118775A true CN1118775A (en) | 1996-03-20 |
Family
ID=5037597
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94115570 Pending CN1118775A (en) | 1994-09-15 | 1994-09-15 | Method for producing solanesol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1118775A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304344C (en) * | 2005-10-09 | 2007-03-14 | 谢兆钟 | Method for recovering solvent from tail gas while extracting solanesol from tobacco |
| CN1305823C (en) * | 2005-10-09 | 2007-03-21 | 谢兆钟 | Energy saving method for extracting solanesol from tobacco |
| US7649120B2 (en) | 2008-02-20 | 2010-01-19 | Northwest Normal University | Microwave-assisted extraction of solanesol from potato stems and/or leaves |
| CN101250560B (en) * | 2008-04-07 | 2011-05-11 | 谢兆钟 | Method for producing alcohol by using tobacco waste |
-
1994
- 1994-09-15 CN CN 94115570 patent/CN1118775A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304344C (en) * | 2005-10-09 | 2007-03-14 | 谢兆钟 | Method for recovering solvent from tail gas while extracting solanesol from tobacco |
| CN1305823C (en) * | 2005-10-09 | 2007-03-21 | 谢兆钟 | Energy saving method for extracting solanesol from tobacco |
| US7649120B2 (en) | 2008-02-20 | 2010-01-19 | Northwest Normal University | Microwave-assisted extraction of solanesol from potato stems and/or leaves |
| CN101250560B (en) * | 2008-04-07 | 2011-05-11 | 谢兆钟 | Method for producing alcohol by using tobacco waste |
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