CN107254351A - Utilize the black efficient method for producing oil of tiger seed - Google Patents
Utilize the black efficient method for producing oil of tiger seed Download PDFInfo
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- CN107254351A CN107254351A CN201710636954.5A CN201710636954A CN107254351A CN 107254351 A CN107254351 A CN 107254351A CN 201710636954 A CN201710636954 A CN 201710636954A CN 107254351 A CN107254351 A CN 107254351A
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- black tiger
- tiger seed
- oil
- liquid
- water
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
Abstract
The present invention provides the black tiger seed of aqueous enzymatic method system oily process, and seed benevolence is ground, adds water, adjusts material liquid pH value, adds mixed enzyme and is digested, and centrifuges to obtain seed oil and waste water；Waste water is handled through 732 cationic exchange resin adsorptions, is recycled multiple；It is raw material to circulate liquefaction wastewater produced, and feed is used for after fermented processing and is added.The method can be such that emulsification substantially weakens, and the content of phenols, saponin(e in water and in oil is decreased obviously, and the circulating repetition of more conducively water is used, and reduces the discharge capacity of waste.Using feed fermentation agent is produced based on waste water, the risk of waste pollution environment can be greatly reduced, while also improving the value of active ingredient in waste.
Description
Technical field
The invention belongs to food processing technology field, it is related to a kind of method that black tiger seed produces black tiger seed oil, specifically
It is related to a kind of aqueous enzymatic method and produces black tiger seed oil and its waste recycling method.
Background technology
Black tiger be called mountain breeze, dust storm rattan, Chinese hydrangeavine root-bark, thoroughly like a chain of pearls or a string of beads, 300 liang of silver, red brill, tonkin pepper herb, enter ground musk deer
Perfume, Mi Duoluo, wammel, orangutan kadsura longepedunculata, ZUANGUFENG, it is infrared disappear, cross bee saage, the thick leaf fruit of Chinese magnoliavine, be it is evergreen climb up by holding on to liana, it is long
3-6m.In the lower portion of the stem deadlock volt soil, top winding, branch cylinder, brownish black, sparsely grow white point-like hole skin.Single leaf alternate；The long 1- of handle
2.5cm；Leaf keratin, blade Long Circle is to ovum shape lanceolar, long 8-17cm, wide 3-8cm, and tip is blunt or anxious sharp, base portion wide wedge shape
Or subcircular, full edge, above bottle green, glossy, several hairless, 6-7 pairs of lateral vein, net vein is not obvious.Spend single leave armpit, it is dilute into
It is right, dioecism；Perianth red or reddish yellow, 10-16 pieces, ellipse or ellipticity obovate, long 12-15mm, wide 5-14mm；
Oecium ellipse or cone, tip have wire to bore shape adjunct；Stamen 14-48, lines up 2-5 row；Gynoecium is avette to ball
Shape, gynoecium 5-7 row.Aggregate fruit is subsphaeroidal, red when ripe or black purple, diameter 6-10cm or bigger；Small berries obovate is long
Up to 4cm, exocarp keratin does not show seed.Seed is red, and heart-shaped or ovate is heart-shaped.The month at florescence 5-7, the fruiting period 8-10 months.Habitat
Branch's ecological environment：It is born in the sparse woods of mountain region, is often wound on big tree.Resource distribution：Be distributed in Jiangxi, it is Fujian, Hunan, wide
The ground such as east, Guangxi, Sichuan, Guizhou, Yunnan.Edible fruit is used, and root can be used as medicine, and its seed can extract oil.
Black tiger seed oil extract method mainly has milling process and extraction.Milling process can keep the flavour of product.
But this method residual oil content height (7-10%), labor intensity is big, cost is high, power consumption is big, and in grouts protein denaturation seriously,
Fertilizer can only be used as, the waste of a large amount of quality plant albumen is caused.By comparison, lixiviation process production efficiency is high and residual oil content is low
(1-4%).But lixiviation process also has weak point：Equipment is more, investment is big；Crude oil complicated component is, it is necessary to strict refining treatment, oil
Product flavor loss is big；The wet dregs of rice are denatured greatly in high temperature desolvation process；For the high oilseed of oil content, using direct leaching
Solvent recovering system load is big；The triviality of technique, the security for reducing production are added using organic solvent, cause ring
The pollution in border；The minim organic solvent remained in product oil is unfavorable to human health.Also have two methods and meanwhile use pre- squeezing-
Lixiviation process, i.e., first extrude the oil of 70-80% in raw material, then remaining oil is extracted with lixiviation process with milling process.It is pre- to squeeze
Although lixiviation process oil extracting rate height (below 1%, powder-material is below 2% for dregs of rice residual oil content), puies forward oily process and causes albumen in various degree
Qualitative change, so that its nutritive value and functional character are influenceed, and extraction process needs desolventizing, equipment is more, and investment is big, pollution
Weight.By contrast, aqueous extraction method mild condition, equipment is simple, environment-friendly, oil quality is high, but because is easier to cause a large amount of
Emulsification cause edible vegetable oil yield not high.
Publication No. CN104606291A Chinese patent discloses a kind of black tiger berry extract as phytoestrogen
New application, take 1 part of dry fruit plus 4~10 times of 95% ethanol, 50~60 DEG C of refluxing extractions are secondary, each 2h, filter, filtrate
Merge, concentrate drying is produced.
Publication No. CN105168520A Chinese patent discloses a kind of preparation method of Caulis Kadsurae Coccineae extract, including with
Lower step：S1. after black tiger is crushed, extracted 1~3 time with 6~12 times of ethanol solutions of volume 50~95%, 1~3h extracted every time,
Filtered after letting cool, merging filtrate is concentrated to give thick paste；S2. thick paste is taken to be suspended in the water of 1~5 times of volume, with 1~3 times of volume stone
Oily ether-ethyl acetate mixed solvent is extracted 1~3 time repeatedly, merges organic solvent extraction layer, recycling design dry, pulverize black
Tiger extract.
Publication No. CN105533746A Chinese patent discloses a kind of preparation method of black tiger instant powder, including with
Lower preparation process：1) take that 80~120 parts by weight do black tiger and 15~30 parts by weight Chinese medicine additives are cleaned respectively, crush；2)
Take half weight to do black tiger to be well mixed with Chinese medicine additive, add the yeast of Chinese medicine additive weight 0.04%~0.08%
Powder and dry black 2~5 times of water of tiger gross weight, stir, are fermented 3~7 days at 20~33 DEG C, obtain fermentate；3) to surplus
Under half weight do black tiger and add and do black 4~6 times of water of tiger gross weight, regulation pH value to 3.5~4.5, temperature is 45~
55 DEG C, the complex enzyme of dry black tiger gross weight 0.3%~0.6% is added, digests 4~7 hours, obtains zymolyte；4) will step
The rapid fermentate 2) obtained and step 3) obtained zymolyte mixes, and homogeneous is dried, obtains black tiger instant powder；Step 3) institute
The complex enzyme stated is that weight ratio is 2:7 pectin lyase and the mixture of cellulase；Described Chinese medicine additive, by following
The raw material of parts by weight is made：40~60 parts of Asian puccoon, 30~50 parts of luffa, 20~40 parts of butterflybush flower, 10~30 parts of Chinese lobelia, soil
5~15 parts of Poria cocos.
Publication No. CN105441268A Chinese patent discloses a kind of brewing method of black tiger Fermented Fruit Wine, bag
Include the following steps：Black tiger fruit is broken into slurry, magma is obtained；By the magma, water and sucrose with 1:2‐4:1-1.5 weight
Than mixing, pH value is adjusted to 3.4-4.3, obtains treating zymotic fluid；Treat to add ferment in zymotic fluid to described by 3-10% weight ratio
Female activating solution, fermentation, then sequentially pass through remove slag, ageing, obtain finished product.
At present, the correlative study of the black tiger seed oil of aqueous enzymatic extraction is had no, after the black tiger seed oil of aqueous enzymatic extraction
Process water be sticky slurries, wherein containing substantial amounts of crude protein, carbohydrate isoreactivity functional component.What is formed is useless
Water not discharge by purified treatment, easily grows putrefactive microorganisms, and especially using acidogenic bactria and mould as very, directly discharge will make to environment
Into pollution.The present invention is fully recycled by the recycling to water and to carbohydrate, amino acid in waste water etc., is from now on
Effective utilize of the oily technique waste water of black tiger seed provides reference.
The content of the invention
Organic solvent, which extracts the oily method of black tiger seed, easily makes chemical substance be remained in black tiger seed oil, causes edible wind
Danger.Market is more willing to use the black tiger seed oil tech products obtained therefrom of aqueous enzymatic extraction, eats the problems such as risk is not present, black tiger
Seed oil quality is higher.But a large amount of industrial wastewaters can be produced during the black tiger seed oil of aqueous enzymatic method system, it is big due to containing in waste water
The antibacterial substances such as the saponin(e of amount, can not thoroughly be solved using conventional waste water processing method, and cause business processes waste water cost
It is very high.In order to make up the defect of prior art, the present invention provides a whole set of black tiger seed oil-producing technique method, and the method also add
Liquefaction formation waste water treatment process, prepares than traditional black tiger seed oil and aqueous enzymatic method oil-producing technique possesses more perfect preparation work
Skill, made black tiger seed oil is more with health role, produces more preferable environment-protecting clean, compensate for the existing oily technique of the black tiger seed of system
Defect, and the market demand for preparing black tiger seed oil on a large scale can be met.
First purpose of the invention is to provide a kind of oily process of the black tiger seed of aqueous enzymatic method system, and it is comprised the following steps that：
(1) black tiger seed is weighed, is ground 1~3 time on common grinding machine, the warm water that water temperature is 30~40 DEG C is added to
In, feed liquid is obtained after stirring；
(2) regulation material liquid pH is 5~6.5, adds amylase and cellulase respectively to final concentration of 30~140U/L, enzyme
Solve certain time；
(3) acid protease (more than 45 DEG C rapid deactivation characteristics) of temperature sensitivity is added again to end into enzymolysis material
Concentration is 50~150U/L, digests certain time, and 20~35min is incubated more than 55 DEG C, feed liquid I is obtained.
(4) feed liquid I is centrifugally separating to obtain liquid and wet slag on sedimentation centrifuge, liquid is directly entered dish-style separation
Machine, isolates black tiger seed oil and waste water I.
(5) filtered after the black tiger seed oil of gained being dried, stood under vacuum, obtain the black tiger seed oil of finished product, and
Examine product oil.
(6) waste water I obtains efflux I through 732 cationic exchange resin adsorptions, and 732 cationic ion-exchange resins are used after absorption
0.3~3mol/L hydrochloric acid is eluted, and obtains eluent.
The reagent of above-mentioned regulation pH value of solution is 0.5moL/L hydrochloric acid or 0.5moL/L sodium hydrate aqueous solutions.
Above-mentioned enzymolysis time is 0.5~4h.
In a specific embodiment, step (1) the volume L for adding water and black tiger seed weight kg ratios are 1
~4：1.
In a specific embodiment, step (6) eluent, is neutralized, high temperature evaporation with 1mol/L sodium hydroxides
Concentration, obtains aminoacids solution, can adjust pH and be refining to obtain various amino acid sterlings, can also be directly used in Plant leaf fertilizer or feeding
Feed additives are used.
Second purpose of the invention is to provide the method for the waste water material recycling that above-mentioned liquefaction is produced, its specific steps
It is as follows：
(a) black tiger seed is weighed, is ground 1~3 time on common grinding machine, efflux I is added, is heated to 30~40 DEG C of left sides
The right side, obtains feed liquid II after stirring；
(b) regulation feed liquid II pH is 5.5~6.5, adds amylase and cellulase respectively to final concentration of 30~100U/
L, digests certain time, obtains enzymolysis liquid I；
(c) acid protease (more than 45 DEG C rapid deactivation characteristics) of temperature sensitivity is added again into enzymolysis liquid I extremely
Final concentration of 40~100U/L, digests certain time, and 20~35min is incubated more than 55 DEG C, feed liquid III is obtained.
(d) feed liquid III is centrifugally separating to obtain liquid and wet slag on sedimentation centrifuge, liquid is directly entered dish-style separation
Machine, isolates black tiger seed oil and waste water II.
(e) filtered after the black tiger seed oil of gained being dried, stood under vacuum, obtain the black tiger seed oil of finished product, and
Examine product oil.
(h) by gained waste water II through 732 cationic exchange resin adsorptions, efflux II is obtained.
(I) by gained efflux II and black tiger seed after grinding, 30~40 DEG C or so are heated to, into enzymolysis next time
Oily circulation step is carried, efflux is circulated 3~5 times and used, the weight kg ratios of the wherein volume L of efflux II and black tiger seed are 10
~15：1.
The reagent of above-mentioned regulation pH value of solution is 0.5moL/L hydrochloric acid or 0.5moL/L sodium hydrate aqueous solutions.
Above-mentioned enzymolysis time is 0.5~4h.
In a specific embodiment, the volume L of step (a) the addition efflux I and black tiger seed weight kg
Than for 6~10：1.
By repeatedly carry oil circulation obtain efflux be acidified, centrifugal treating, clear liquid can directly high temperature evaporation obtain
Glucose crude product.
3rd purpose of the invention is to provide the method for the wastewater produced production feed fermentation agent of above-mentioned circulation liquefaction, specifically
Step includes as follows：Wastewater produced circulation liquefaction is raw material (needing not move through the processing of 732 cationic exchange resin adsorptions), plus
Enter mass ratio for 10~20% bacillus subtilis powders, 30~40 DEG C of aerobic fermentation 12~36h of culture are refrigerated at 0~5 DEG C and made
30~35 DEG C of low temperature dryings are standby after directly using or mixed with beancake powder and corn flour mixed fodder for feed fermentation agent.
The above-mentioned bacillus subtilis that uses is the feed that can directly be bought with market with bacillus subtilis, and can be produced
The bacterial strain of neutral proteinase.
Technique effect
1st, emulsification of the protein during the oil separation of black tiger seed is avoided, enables black tiger seed oil quickly and water
Separation, is also remarkably decreased black tiger seed oil and Phenol for Waste Water class, the content of saponin(e；Improve amino acid and monose in waste water
Content, is also beneficial to waste water and can return to reuse 2~4 times.
2nd, due to reducing protein content during black tiger seed oil is extracted, emulsification is made substantially to weaken, phenols,
The content of saponin(e in water and in oil is decreased obviously, and the circulating repetition of more conducively water is used, and reduces the discharge capacity of waste water.
3rd, due to directly using feed fermentation agent is produced based on waste water, the wind of contaminated wastewater environment can be greatly reduced
Danger, while also improving the value of active ingredient in waste water.
Embodiment
Embodiment 1
Black tiger seed 100kg is weighed, is ground 1~3 time on common grinding machine, the warm water that water temperature is 30~40 DEG C is added to
In 300L, feed liquid is obtained after stirring；It is 6 with 0.5moL/L hydrochloric acid or 0.5moL/L sodium hydrate aqueous solutions regulation material liquid pH,
Amylase and cellulase extremely final concentration of 90U/L or so respectively are added, 4h is digested.It is sensitive that temperature is added again into enzymolysis material
Property acid protease (more than 45 DEG C rapid deactivation characteristics) to final concentration of 100U/L, digest 3h, be incubated more than 55 DEG C
35min, obtains feed liquid I.Feed liquid I is centrifugally separating to obtain liquid and wet slag on sedimentation centrifuge, liquid is directly entered dish-style point
Disembark, isolate black tiger seed oil and waste water I.Filter, obtain after the black tiger seed oil of gained is dried, stood under vacuum
The black tiger seed oil of finished product, and examine product oil.Waste water I obtains efflux I through 732 cationic exchange resin adsorptions, 732 after absorption
Cationic ion-exchange resin is eluted with 0.3~3mol/L hydrochloric acid, obtains eluent.
Embodiment 2
Black tiger seed 200kg is weighed, is ground 3 times on common grinding machine, 1500L effluxes I is added, is heated to 30~40
DEG C or so, feed liquid II is obtained after stirring；It is with 0.5moL/L hydrochloric acid or 0.5moL/L sodium hydrate aqueous solutions regulation material liquid pH
5.5, amylase and cellulase are added respectively to final concentration of 75U/L, digest 3h.Add temperature again into enzymolysis liquid I quick
The acid protease (more than 45 DEG C rapid deactivation characteristics) of perception digests 3h to final concentration of 110U/L, is incubated more than 55 DEG C
35min, obtains feed liquid III.Feed liquid III is centrifugally separating to obtain liquid and wet slag on sedimentation centrifuge, liquid is directly entered dish-style
Seperator, isolates black tiger seed oil and waste water II.Filtered after the black tiger seed oil of gained is dried, stood under vacuum,
The black tiger seed oil of finished product is obtained, and examines product oil.By gained waste water II through 732 cationic exchange resin adsorptions, efflux is obtained
Ⅱ.By the 2500L of gained efflux II and black tiger seed 200kg after grinding, 30~40 DEG C or so are heated to, into enzyme next time
Solution carries oily circulation step, and efflux is circulated 3~5 times and used.
Embodiment 3
It is raw material to take wastewater produced (without the resin treatment) 500kg of circulation liquefaction, adds 75kg bacillus subtilis powders
(15%), 37 DEG C of culture 24h, are used directly in refrigerate at 0~5 DEG C and are directly used as feed fermentation agent, after measured total amino acid
Content 105mg/g, proteinase activity reaches 1340U/g.
Claims (7)
1. a kind of oily process of the black tiger seed of aqueous enzymatic method system, it is comprised the following steps that：
(1) black tiger seed is weighed, is ground 1~3 time on common grinding machine, is added in the warm water that water temperature is 30~40 DEG C, stirs
Feed liquid is obtained after mixing uniformly；
(2) regulation material liquid pH is 5~6.5, adds amylase and cellulase respectively to final concentration of 30~140U/L, enzymolysis one
Fix time；
(3) acid protease (more than 45 DEG C rapid deactivation characteristics) of temperature sensitivity is added again to final concentration into enzymolysis material
For 50~150U/L, certain time is digested, 20~35min is incubated more than 55 DEG C, feed liquid I is obtained.
(4) feed liquid I is centrifugally separating to obtain liquid and wet slag on sedimentation centrifuge, liquid is directly entered disk centrifuge, point
Separate out black tiger seed oil and waste water I.
(5) filtered after the black tiger seed oil of gained being dried, stood under vacuum, obtain the black tiger seed oil of finished product, and examine
Product oil.
(6) waste water I obtains efflux I through 732 cationic exchange resin adsorptions, after absorption 732 cationic ion-exchange resins with 0.3~
3mol/L hydrochloric acid is eluted, and obtains eluent.
2. method according to claim 1, wherein enzymolysis time are 0.5~4h.
3. method according to claim 1, wherein step (1) the volume L for adding water and black tiger seed weight kg ratios are 1
~4：1.
4. the method that the waste water material that a kind of black tiger seed oil of aqueous enzymatic method system is produced is recycled, it is comprised the following steps that：
(a) black tiger seed is weighed, is ground 1~3 time on common grinding machine, efflux I is added, is heated to 30~40 DEG C or so,
Feed liquid II is obtained after stirring；
(b) regulation feed liquid II pH is 5.5~6.5, adds amylase and cellulase respectively to final concentration of 30~100U/L, enzyme
Certain time is solved, enzymolysis liquid I is obtained；
(c) acid protease (more than 45 DEG C rapid deactivation characteristics) for adding temperature sensitivity again into enzymolysis liquid I is dense to end
Spend for 40~100U/L, digest certain time, 20~35min is incubated more than 55 DEG C, feed liquid III is obtained；
(d) feed liquid III is centrifugally separating to obtain liquid and wet slag on sedimentation centrifuge, liquid is directly entered disk centrifuge, point
Separate out black tiger seed oil and waste water II；
(e) filtered after the black tiger seed oil of gained being dried, stood under vacuum, obtain the black tiger seed oil of finished product, and examine
Product oil；
(h) by gained waste water II through 732 cationic exchange resin adsorptions, efflux II is obtained；
(I) by gained efflux II and black tiger seed after grinding, 30~40 DEG C or so is heated to, oil is carried into enzymolysis next time
Circulation step, efflux is circulated and used for 3~5 times, the weight kg ratios of the wherein volume L of efflux II and black tiger seed for 10~
15：1.
5. method according to claim 4, wherein enzymolysis time are 0.5~4h.
6. the volume L of method according to claim 4, wherein step (a) the addition efflux I and black tiger seed weight kg
Than for 6~10：1.
7. a kind of method of the wastewater produced production feed fermentation agent of aqueous enzymatic method circulation liquefaction, specific steps include as follows：Circulation
Wastewater produced liquefaction is raw material, and addition mass ratio is 10~20% bacillus subtilis powders, 30~40 DEG C of aerobic fermentation cultures
12~36h, refrigerates at 0~5 DEG C and directly uses or mixed with beancake powder and corn flour mixed fodder as feed fermentation agent
30~35 DEG C of low temperature dryings are standby after conjunction.
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| CN108553391A (en) * | 2018-07-01 | 2018-09-21 | 佛山文森特知识产权服务有限公司 | A kind of preparation method of the plant fermentation composition with anti-wrinkle |
| CN112143556A (en) * | 2020-09-16 | 2020-12-29 | 湖南农业大学 | Preparation method of bitter-free black tiger seeds and seed oil |
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Application publication date: 20171017 |