CN102321384A - Liquid-phase supercritical method for removing and separating spiciness from capsicum red pigment and device special for liquid-phase critical method - Google Patents

Liquid-phase supercritical method for removing and separating spiciness from capsicum red pigment and device special for liquid-phase critical method Download PDF

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CN102321384A
CN102321384A CN201110167777A CN201110167777A CN102321384A CN 102321384 A CN102321384 A CN 102321384A CN 201110167777 A CN201110167777 A CN 201110167777A CN 201110167777 A CN201110167777 A CN 201110167777A CN 102321384 A CN102321384 A CN 102321384A
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liquid
extracting rectifying
capsicum
separator
red pigment
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CN102321384B (en
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王玉琪
侯磊磊
马亚峰
郑岚
陈开勋
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Shanxi Yunyidao Biotechnology Co ltd
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Northwest University
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Abstract

The invention discloses a liquid-phase supercritical method for removing and separating spiciness from capsicum red pigment, which comprises the following steps of: allowing liquid capsicum resin serving as a raw material to flow down from upper part of an extractive distillation column through a material inlet and a liquid distributor, introducing supercritical CO2 through a CO2 gas inlet at the bottom of the extractive distillation column, and performing countercurrent extraction; discharging an extract through an extract outlet on the top of the extractive distillation column, and introducing into a separator I and a separator II in turn to remove an organic solvent and a capsicum element; and discharging raffinate of a pure capsicum red pigment product through a raffinate outlet at the bottom of the extractive distillation column, and collecting. The raw material and an extracting agent are in countercurrent contact, and the mass transfer effect is enhanced; continuous production can be realized and the production efficiency is improved; and the liquid capsicum resin with low color value, which is prepared by a solvent method, is taken as a raw material, and the capsicum red pigment product of which the color value is improved from 80 of the raw material to more than 320 can be obtained.

Description

Overcritical removing spiciness from capsicum red pigment separation method of a kind of liquid phase and isolated plant thereof
Technical field
The present invention relates to overcritical removing spiciness from capsicum red pigment separation method of a kind of liquid phase and isolated plant thereof, the continuous extraction that can be applicable to CAPSAICIN with separate, and can be to the tail gas clean-up recycle.
Background technology
Supercritical liquid extraction technique is a kind of new separation technology that rises in the last thirty years; In food, makeup, medicine, active ingredient of natural plant extraction and field of petrochemical industry increasingly extensive application is arranged, and obtained a series of industrial applications achievements.Wherein supercritical co has that dissolving power is strong, rate of mass transfer is high, suitable (the emergent pressure 7.3MPa of critical parameter; Plurality of advantages such as 31 ℃ of critical temperatures), unreactiveness, nontoxic, no burn into be cheap and easy to get and safe and efficient; Make the supercritical extraction sepn process can be near conveniently carrying out under the room temperature condition, and make carbonic acid gas become the supercritical fluid solvent of suitable industrial applications.Therefore, the research of supercritical carbon dioxide extraction method and application facet have all obtained very big development in recent years.
The CAPSAICIN color and luster is delicious, has no side effect, and has very high biological value, is classified as category-A food dye by the Food and Argriculture OrganizationFAO and the World Health Organization.In recent years; Along with the toxic continuous discovery of synthetic colour; The synthetic colour that use countries in the world reduces day by day, and CAPSAICIN except that food service industry is used, all has very widely use in industries such as makeup, beverage candy, medicine, feeds as Green Product.Mostly the method for producing CAPSAICIN now is solvent method, and the CAPSAICIN dissolvent residual that this method is produced is many, and peculiar smell is arranged, and the look valency is low, and there are shortcomings such as solvent recuperation is difficult, energy consumption is big, extraction yield is low in technological process.In recent years, along with the development of supercritical carbon dioxide extraction method, the existing supercritical carbon dioxide extraction method that adopts is to CAPSAICIN extraction, isolating relevant report.
As: the ZL99114740.5 patented claim discloses a kind of supercritical CO 2 refining process of deodored capsanthin; This method key step comprises that extraction, flash trapping stage, secondary separate; Promptly will not take off peppery earlier or taken off peppery CAPSAICIN through being pumped in the extractor; Then with being pumped into supercritical carbon dioxide fluid and organic solvent (ethanol, acetone or isopropyl acetone); Regulate the extractor pressure and temperature different and extract, obtain the purified CAPSAICIN in the last extractor, obtain isolate in the separating still with separating still.But this method adopts periodical operation, can not realize continuous production, and production efficiency is low; And this method is a raw material with the thick product of the higher CAPSAICIN of cost, and the look valency is promoted to farthest 260 by 150 after carrying the agent supercritical extraction, and the look valency lifting rate of CAPSAICIN product is lower; Carry agent owing to add ethanol, isopropyl acetone etc. in the extraction separation process in addition, caused higher organic solvent residual in the CAPSAICIN product.
Summary of the invention
Technical problem to be solved by this invention is, a kind of defective that can overcome prior art is provided, and realizes extraction, separates, purifies integrated quantity-produced performance liquid CAPSAICIN supercritical extraction and take off peppery device.
The present invention is an extraction feed with the liquid capsicum resin, and described liquid capsicum resin is that the chilli mature fruit uses organic solvent (sherwood oil, acetone or alcohol) extraction to get after crushed.Mainly contain CAPSAICIN, pungent plain (capsicine) and organic solvent in the liquid capsicum resin, wherein supercritical co can dissolve pungent element and the organic solvent in the liquid capsicum resin.
The present invention addresses the above problem the technical scheme that is adopted:
The overcritical removing spiciness from capsicum red pigment separation method of a kind of liquid phase may further comprise the steps:
(1) be raw material with the liquid capsicum resin, capsicum resin flows down supercritical CO through material inlet and liquid distributor (5) from extracting rectifying post (F) top 2CO from extracting rectifying post (F) bottom 2Gas feed (7) gets into, and carries out counter-current extraction; (2) extract (is dissolved with the CO of pungent element and organic solvent 2) extract outlet (1) discharge from extracting rectifying post (F) top, get into separator successively
Figure 943569DEST_PATH_IMAGE001
(G) and separator
Figure 329551DEST_PATH_IMAGE002
(H) remove organic solvent and pungent element;
(3) the pure CAPSAICIN product of extract remainder is discharged and is collected from extracting rectifying post (F) bottom extract remainder material outlet (8).
In the above-mentioned steps (2), CO 2Tail gas takes off peppery device (I), and to remove in the gas phase dissolved pungent plain, removes the CO behind the pungent element 2Reusable edible.
The working pressure of above-mentioned extracting rectifying post (F) is 10-30MPa, and service temperature is 35-80 ℃; The pressure of separator I (G) is 5-10MPa, and temperature is 35-80 ℃; Control separator II (H) and CO 2The pressure that tail gas takes off peppery device (I) is 4-8MPa, and temperature is 35-80 ℃; Liquid capsicum resin inlet amount is 2-8L/h, CO 2Circular flow is 5-40L/h.
The isolated plant of the overcritical removing spiciness from capsicum red pigment separation method of above-mentioned liquid phase comprises extraction plant and tripping device, wherein extracting rectifying post (F) and separator
Figure 109289DEST_PATH_IMAGE001
(G), separator
Figure 724072DEST_PATH_IMAGE002
(H) and CO 2Tail gas takes off peppery device (I) connects successively, and extracting rectifying post (F) bottom is provided with CO 2Gas feed (7) and extract remainder material outlet (8), the top is provided with extract outlet (1).
The cylindrical shell (9) of extracting rectifying post (F) is divided into three sections of upper, middle and lower, and every section all is provided with material inlet and liquid distributor (5), and liquid material can adopt three sections chargings individually or simultaneously; The cylindrical shell (9) of extracting rectifying post (F) is provided with the three sections chucks in upper, middle and lower (10); Feed heat transferring medium in each section chuck (10); Heat transferring medium is got into by heat transferring medium import (6); Leave from heat transferring medium outlet (11), each section temperature can be regulated and control separately, and can extraction temperature be set according to different technology conditions; Regular wire cloth or ripple packing (4) are housed in the cylindrical shell (9) of extracting rectifying post (F); The maximum operating pressure of extracting rectifying post (F) is 50MPa, and top temperature is 300 ℃, and material is a stainless steel; Be provided with mist eliminator (2), hold-down grid (3), liquid re-distributor (12) and supporting plate (13) in the extracting rectifying post (F).
Described CO 2It is a hollow cylinder tank body that tail gas takes off peppery device (I), interior dress different activities spicy-off agency, and maximum withstand voltage 30MPa, maximum operating temperature is 100 ℃, material is a stainless steel.
The present invention compared with prior art has the following advantages and beneficial effect:
(1) the present invention makes raw material and extraction agent counter current contact, has strengthened mass transfer effect, and can realize continuous production, has improved production efficiency.(2) the present invention is that the liquid capsicum resin of the low look valency of employing solvent method gained is a raw material, and look valency lifting rate is very high.After apparatus of the present invention processing, can obtain the look valency and bring up to the CAPSAICIN product more than 320 by 80 of raw material.(3) the present invention separates and takes off in the peppery purification process process at whole supercritical extraction, does not add any organic solvent and carries agent, and products obtained therefrom is no more than 10ppm through detecting Determination of Residual Organic Solvents, far below the national standard of organic residual 25ppm.(4) the present invention has designed CO 2Take off peppery device, when having reduced pigment product pungent cellulose content, tail gas is done further purifying treatment, solved the higher difficult problem that makes pigment product have pungent of pungent cellulose content in the tail gas, realize CO 2The recycle of gas, energy-conserving and environment-protective and reducing cost.
Description of drawings
Fig. 1 is a process flow sheet of the present invention;
A is CO among the figure 2Storage tank, B are ice chest, and C is a force (forcing) pump, and D is a raw material storage tank, and E is a charge pump, and F is the extracting rectifying post, and G is the separator I, and H is the separator II, and I is CO 2Take off peppery device.
Fig. 2 is the structure iron of extracting rectifying post;
1 is the extract outlet among Fig. 2, and 2 is mist eliminator, and 3 is hold-down grid, and 4 is filler, and 5 is material inlet and liquid distributor, and 6 is the heat transferring medium import, and 7 is CO 2Gas feed, 8 are the outlet of extract remainder material, and 9 is extracting rectifying column casing body, and 10 is chuck, and 11 are the heat transferring medium outlet, and 12 is liquid re-distributor, and 13 is supporting plate.
Embodiment
Do further description through the embodiment specific embodiments of the invention below, therefore do not limit the present invention among the described scope of embodiments.
Embodiment 1 is a raw material with solvent method gained liquid capsicum resin midbody, adopts apparatus of the present invention to obtain high luminance relay valency CAPSAICIN.
The high 255cm of the used extracting rectifying post of present embodiment, the filler in the extracting rectifying post is regular wire cloth, the pressure of extracting rectifying post is 50MPa.
Process flow sheet is as shown in Figure 1, and the structure iron of extracting rectifying post is as shown in Figure 2, CO 2By CO 2Storage tank (A) is pressurized to 10-30MPa through force (forcing) pump (C) after getting into ice chest (B) cooling, and extracting rectifying post (F) temperature is controlled at 35-80 ℃, gets into the CO in the extracting rectifying post (F) 2Reach supercritical state.
The raw material capsicum resin is got in the extracting rectifying post (F) from extracting rectifying post (F) top through charge pump (E) by raw material storage tank (D), and feed rate is controlled at 2-8L/h.Simultaneously, high pressure CO 2Get into from extracting rectifying post (F) bottom, under supercritical state, carry out counter-current extraction, the control supercritical CO with capsicum resin 2The operation flow be 5-40L/h, working pressure is 10-30MPa.The products obtained therefrom CAPSAICIN is emitted and is collected by extracting rectifying post (F) bottom valve, regulates this valve emission flow is equated with feed rate basically.Extraction products such as pungent element are by supercritical CO 2The dissolving back is taken out of from extracting rectifying post (F) top, gets into the separator I through the variable valve top.
The pressure of separator I is 5-10MPa, and temperature is 35-80 ℃.Separating prod is emitted and is collected, CO by separator I bottom valve 2Fluid gets into the separator II through variable valve from the top.
The pressure of separator II is 4-8MPa, and temperature is 35-80 ℃.Separating prod is emitted and is collected, CO by separator II bottom valve 2Fluid gets into CO through variable valve from the bottom 2Take off peppery device.
CO 2Take off peppery device (I) and removed CO 2Pungent in the fluid is plain, and the pungent element is by CO 2Taking off peppery device (I) bottom valve emits and collects, the CO after the purification 2Turn back to the recycle of gas phase storage tank.
The pure CAPSAICIN product look valency that adopts the extraction of separation method of the present invention and isolated plant is up to 320, and the pungent cellulose content is lower than 0.35%, and the total organic solvent residual volume is lower than 20ppm.Each item leading indicator all is superior to the national standard (GB10783-2008) of CAPSAICIN product.

Claims (10)

1. overcritical removing spiciness from capsicum red pigment separation method of liquid phase may further comprise the steps:
(1) be raw material with the liquid capsicum resin, capsicum resin flows down supercritical CO through material inlet and liquid distributor (5) from extracting rectifying post (F) top 2CO from extracting rectifying post (F) bottom 2Gas feed (7) gets into, and carries out counter-current extraction;
(2) extract from extracting rectifying post (F) top extract outlet (1) discharge, get into separator successively and (G) (H) remove organic solvent and pungent element with separator
Figure 64857DEST_PATH_IMAGE002
;
(3) the pure CAPSAICIN product of extract remainder is discharged and is collected from extracting rectifying post (F) bottom extract remainder material outlet (8).
2. the overcritical removing spiciness from capsicum red pigment separation method of liquid phase according to claim 1 is characterized in that: in the step (2), and CO 2Tail gas takes off peppery device (I), and to remove in the gas phase dissolved pungent plain, removes the CO behind the pungent element 2Reusable edible.
3. the overcritical removing spiciness from capsicum red pigment separation method of liquid phase according to claim 1 is characterized in that: the working pressure of extracting rectifying post (F) is 10-30MPa, and service temperature is 35-80 ℃; The pressure of separator I (G) is 5-10MPa, and temperature is 35-80 ℃; Control separator II (H) and CO 2The pressure that tail gas takes off peppery device (I) is 4-8MPa, and temperature is 35-80 ℃.
4. the isolated plant of the overcritical removing spiciness from capsicum red pigment separation method of the said liquid phase of claim 1 comprises extraction plant and tripping device, it is characterized in that: extracting rectifying post (F) and separator
Figure 175725DEST_PATH_IMAGE001
(G), separator
Figure 465892DEST_PATH_IMAGE002
(H) and CO 2Tail gas takes off peppery device (I) connects successively, and extracting rectifying post (F) bottom is provided with CO 2Gas feed (7) and extract remainder material outlet (8), the top is provided with extract outlet (1).
5. isolated plant according to claim 4 is characterized in that: the cylindrical shell (9) of extracting rectifying post (F) is divided into three sections of upper, middle and lower, and every section all is provided with material inlet and liquid distributor (5), and liquid material adopts three sections chargings individually or simultaneously.
6. isolated plant according to claim 5; It is characterized in that: the cylindrical shell (9) of extracting rectifying post (F) is provided with the three sections chucks in upper, middle and lower (10); Feed heat transferring medium in each section chuck (10), heat transferring medium is got into by heat transferring medium import (6), leaves from heat transferring medium outlet (11); Each section temperature is regulated and control separately, according to different technology conditions extraction temperature is set.
7. isolated plant according to claim 6 is characterized in that: regular wire cloth or ripple packing (4) are housed in the cylindrical shell (9) of extracting rectifying post (F).
8. isolated plant according to claim 4 is characterized in that: the maximum operating pressure of extracting rectifying post (F) is 50MPa, and top temperature is 300 ℃, and material is a stainless steel.
9. isolated plant according to claim 4 is characterized in that: be provided with mist eliminator (2), hold-down grid (3), liquid re-distributor (12) and supporting plate (13) in the extracting rectifying post (F).
10. isolated plant according to claim 4 is characterized in that: described CO 2It is a hollow cylinder tank body that tail gas takes off peppery device (I), interior dress different activities spicy-off agency, and maximum withstand voltage 30MPa, maximum operating temperature is 100 ℃, material is a stainless steel.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104530748A (en) * 2014-11-27 2015-04-22 安徽省万顺现代农业科技有限公司 Method for extracting capsicum haematochrome from capsicum
CN107594472A (en) * 2017-10-30 2018-01-19 潍坊友容实业有限公司 A kind of Suaeda salsa biogenic salt and Betacyanins combined extraction method
CN108440989A (en) * 2018-03-20 2018-08-24 何冠阅 A kind of green basic material preparation facilities

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104530748A (en) * 2014-11-27 2015-04-22 安徽省万顺现代农业科技有限公司 Method for extracting capsicum haematochrome from capsicum
CN107594472A (en) * 2017-10-30 2018-01-19 潍坊友容实业有限公司 A kind of Suaeda salsa biogenic salt and Betacyanins combined extraction method
CN108440989A (en) * 2018-03-20 2018-08-24 何冠阅 A kind of green basic material preparation facilities

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