CN1047773C - Method for preparation of natural carotene - Google Patents

Abstract

The present invention relates to a preparation method of natural carotene. After dunaliella salina is cultivated for 7 to 10 days, an obtained algae liquid is mixed with an iron trichloride solution and dissolved air water by an air floatation method to obtain an algae paste, and the algae paste is directly extracted and purified to prepare carotene crystals and a concentrated extract liquid product. An extraction agent is ethyl acetate which is an edible organic solvent, a closed extraction process is adopted, dreg harrowing by opening a door is not needed, work situation is improved, complicated algae paste processing technologies are eliminated in the whole process, and a large number of apparatuses, factory buildings and energy sources are saved; thus, the preparation method has low production cost and high product quality. Compared with a product prepared by using an old freezing method, the content of alpha-carotene in the crystal product, and the concentrated extract liquid product is increased by 10%. The preparation method has the advantages of simple technology, low cost, low energy consumption and improved work situation; the preparation method is suitable for large-scale industrial production.

Description

The preparation method of natural Beta-carotene

The present invention relates to from the salt algae, extract the processing method of natural Beta-carotene.

The existing method of extracting natural Beta-carotene from the salt algae has two classes, and a class is to enter the molten product of extraction process Separation and Recovery carotin oil after the salt algae is concentrated, and is called liquid extraction, as US4680314; Another kind of is dry method, the salt algae that is about to concentrate is processed into xeraphium and carries out extracting and separating again, as CN1044277A " extracting method of carotene in the salt algae ", CN1059715A " method and apparatus of leaching carotene from the salt algae ", CN1059716A " method of leaching carotene from the salt algae " etc., the algae of concentrating in the above-mentioned patent is stuck with paste must be through washing and desalting, centrifuge dehydration, freezing, one's water breaks algae are also melted with steam, operation such as centrifugation, vacuum-drying is made sand shape algae powder again, and operations such as the algae powder extracts again, separation prepare the carotene product.The wet method of the first kind prepares in the carotene process, complex compounds such as Tiorco 677 salt commonly used expensive, molysite are as the flocculation agent salt algae of concentrating, adding acid in the extraction process makes PH become acid, purpose is to make the dense algae thing of flocculation agent complexing separate complexing, make the salt algae enter oil phase and be extracted, reclaim flocculation agent simultaneously, also necessary alkaline saponification in the operation afterwards, i.e. neutralization is acid, and such processing step is complicated; Second class methods, algae paste into sand shape algae powder, have wasted a large amount of energy and equipment, and must open aperture of door rake slag in the extraction process, solvent evaporates, and work situation is very poor.

The object of the invention provides a kind of work simplification, cost is low and the preparation method of the natural Beta-carotene that Working environment is good.

With reference to accompanying drawing, the preparation method of natural Beta-carotene of the present invention realizes like this, it mainly concentrates the deduction operation of making algae paste operation, algae paste extracting and separating operation, extraction liquid crystallization combinations body carotene and concentrated solution product sequence and separating the slag slurry by algae liquid forms, and it is characterized in that:

1, algae liquid system algae is stuck with paste operation:

A. algae liquid (1) floats with volume ratio mixed stability in mixed processes of liquor ferri trichloridi (4) with 1: 0.006;

B. mixed solution feeds dissolved air water at separation circuit (3), and mixed solution and dissolved air water volume ratio are 70: 30, gets algae through the static separation in separatory basin (7) of the parting liquid after the dissolved air flotation and sticks with paste (8);

2, extraction process: algae is stuck with paste (8) and directly enters extraction process (9), adopts ethyl acetate to make extraction agent, and algae is stuck with paste: ethyl acetate=1: 0.5～1 (volume ratio), 40～50 ℃ of extraction temperature, 30～50 minutes/time extraction time;

3, single extraction liquid (12) is through conventional technology combinations body carotene product (24) and concentrated solution product (26), wherein Tc is 5～-5 ℃;

4, slag slurry deduction operation: slag slurry (13) obtains secondary slag slurry (15) through the extracting and separating operation second time (14), and secondary slag slurry reclaims rectifying liquid (18) in rectification working process (16) rectifying.

Accompanying drawing is the embodiment process flow diagram.

In conjunction with example technical solution of the present invention is described further.

From the salt algae content of culturing the pond is that 10-50 ten thousand cell strain/milliliters or carotene water body content are 2-15g/m ³Algae liquid (1) be pumped to mixed processes (2), the pumping liquid measure is 50-70m ³/ h, adding concentration is 5% FeCl in mixing tank ₃Solution makes algae liquid and FeCl ₃The liquor capacity ratio is 1: 0.006, mixed solution becomes the stable come-up of algae iron floss in mixing device, floss enters air flotation slot separator (3) together with liquid, in separator, feed dissolved air water, make algae iron mixed solution: dissolved air water=70: 30 (volume ratio), the steam pearl that algae iron floss is discharged by dissolved air water in separator is held come-up, reach the purpose of floss and water sepn, isolated water enters back pool (6) and recycles, isolated algae iron floss enters separatory basin (7), the static placement isolated a part of free-water again, and the algae iron mixture that enrichment is closed is the carotene water-content and reaches 500-800g/m ³Algae stick with paste (8) because algae is stuck with paste the static placement through the separatory basin, make algae stick with paste the water content that keeps stable, so that algae is stuck with paste quality is uniform and stable.

Described algae is stuck with paste (8) and directly enters extraction process (9), add ethyl acetate and make extraction agent, algae is stuck with paste and the ethyl acetate volume ratio is 1: 0.5～1, extraction temperature 40-50 ℃, 30～50 minutes/time extraction time, it is extraction liquid (12) and slag slurry (13) that the extraction slurries are isolated clear liquid through separation factor greater than 2700 decanter type separating machine (11), the slag slurry enters extracting and separating operation (14) for the second time, extraction conditions is with for the first time, separate secondary screenings (15) enter rectification working process (16), rectifying tower adopts the filler distillation tower, rectification temperature is 70-90 ℃, rectifying liquid (18) and extraction fluid (17) that rectification working process comes out recycle in extraction process, and rectifying slag (19) promptly can be used as feed and uses.

The described extraction liquid first time (12) filters (19) through conventional processing sequence, evaporation (20), vaporizer adopts thin-film evaporator, vaporizer inner vapor pressure≤0.5MPa, inlet amount is 200L/h, the steam condensate that vaporizer comes out (22) is returned extraction process and is recycled, the dope that vaporizer comes out enters Crystallization Procedure (21), crystallizer adopts jacketed type, in chuck, send low-temperature receiver with refrigerator, the Tc of crystallizer is 5～-5 ℃, the brilliant liquid mixed solution that comes out from crystallizer enters filtration operation (23), isolate crystal carotene product (24), filtered liquid evaporates through evaporating kettle (25), the evaporating kettle Heating temperature is 70-90 ℃, obtains concentrated solution product (26).

The quality product excellence of the existing cold method of the preparation method's gained crystal carotene of natural Beta-carotene of the present invention and the mass ratio of concentrated solution product many.

Institute for drug control, Hainan Province " contains carotene (C to the crystalline content analytical results of this patent method carotene crystal product ₄₀H ₅₆) be 91.63%, analyze May 3 95 year date, to concentrated solution medicinal extract product carotene carotene content analytical results: " contain carotene (C ₄₀H ₅₆) be 16.5%, analyze April 18 94 year date.Above-mentioned analytical results has illustrated that carotene carotene content is all higher in this patent method gained crystal and the concentrated solution product.

Table 1 is the carotene classification analysis data of crystal carotene and concentrated solution product:

Annotate: α-C refers to alpha-carotene

The trans finger transconfiguration of β-c β-Hu Luobusu

β-c cis refers to the cis-structure β-Hu Luobusu

Report according to the parties concerned, α-C oxidation-resistance, anti-cancer ability are than strong ten times of β-Hu Luobusus, from above-mentioned grouped data comparative result, in crystal product, alpha-carotene content this patent method is 21.7%, higher more than 10% than prior art cold method 10.9%, in the concentrated solution product, alpha-carotene content 30.25% is also much higher than cold method.

The preparation method of natural Beta-carotene of the present invention has following characteristics:

1, the salt algae is gathered and adopts the floating type static mixing method, makes the hydrolysis ferric trichloride easily form network, shape Become algae iron floccule come-up to be beneficial to the enrichment frond, can improve recovery ratio, recovery ratio reaches more than 80% in the practice, Ferric trichloride enters during the course in the slag slurry and enters at last in the rectifying slag, has saved acidifying and soap in the whole process Metallization processes;

2, algae is stuck with paste and directly to enter extraction process, saves algae and sticks with paste treatment system, namely saved the washing and depositing device, Sedimentation centrifuge, quick-frozen purl machine, freezer, vaporize algae equipment, centrifugal dehydrator, vacuum drier etc. A series of large-scale process equipments and factory building can be saved about 30-50% such as investment and running expense, saving energy consumption cost, Can save manpower 30%, improve accordingly work efficiency, decrease cost;

3, extractant adopts edible organic solvent-ethyl acetate, is operating as closed, does not adopt oil Slag operation and abominable production environment are not harrowed in the harm of ether and other organic solvent extracts;

4, the algae-residue reextraction has increased distillation system after separating, and has further reclaimed extractant;

5, product quality is superior, and especially alpha-carotene content is than freezing height, and medicinal effects is remarkable.

In sum, the preparation method of natural Beta-carotene of the present invention is the Hu trailing plants from enrichment salt algae to product crystal One cover complete process method of Bu Su, concentrate and rectifying slag, extractant has obtained following fully during the course Ring uses, the product quality excellence, and its whole work simplification, energy consumption is low, equipment investment is low thereby cost Low, operating condition is good simultaneously, so this method is suitable for heavy industrialization.

Claims (1)

1, a kind of preparation method of natural Beta-carotene, it mainly concentrates the deduction operation of making algae paste operation, algae paste extracting and separating operation, extraction liquid crystallization combinations body carotene and concentrated solution product sequence and separating the slag slurry by algae liquid forms, and it is characterized in that:

(1) algae liquid system algae is stuck with paste operation:

A. algae liquid (1) mixes in mixed processes (2) with 1: 0.006 volume ratio with liquor ferri trichloridi (4);

B. mixed solution feeds dissolved air water at separation circuit (3), and the volume ratio of mixed solution and dissolved air water is 70: 30, gets algae through the static separation in a minute liquid storage tank (7) of the parting liquid after the dissolved air flotation and sticks with paste (8);

(2) extraction process:

Algae is stuck with paste (8) and enters extraction process (9), adopts ethyl acetate to make extraction agent, and algae is stuck with paste and the volume ratio of ethyl acetate is 1: 0.5～1,40～50 ℃ of extraction temperature, 30～50 minutes/time extraction time;

(3) single extraction liquid (12) is through conventional technology combinations body carotene product (24) and concentrated solution product (26), and wherein the Tc of Crystallization Procedure is 5～-5 ℃;

(4) slag slurry deduction operation:

Slag slurry (13) obtains secondary slag slurry (15) through the extracting and separating operation second time (14), and secondary slag slurry reclaims rectifying liquid (18) in rectification working process (16) rectifying.