CN101214031B - Comprehensive utilization of seeding-watermelon and method for extracting pectin from seeding-watermelon - Google Patents
Comprehensive utilization of seeding-watermelon and method for extracting pectin from seeding-watermelon Download PDFInfo
- Publication number
- CN101214031B CN101214031B CN2007101800574A CN200710180057A CN101214031B CN 101214031 B CN101214031 B CN 101214031B CN 2007101800574 A CN2007101800574 A CN 2007101800574A CN 200710180057 A CN200710180057 A CN 200710180057A CN 101214031 B CN101214031 B CN 101214031B
- Authority
- CN
- China
- Prior art keywords
- pectin
- watermelon
- value
- acid
- add
- 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.)
- Expired - Fee Related
Links
Abstract
The invention discloses a multiple usage method of seeding watermelon and a method of extracting pectin from the seeding watermelon. The extraction method is that extracting the pectin from the seeding watermelon which is the chief raw material, comprising a plurality of technological chains of raw material collection, pretreatment, acid extraction, leaching, enrichment, alcohol extraction, drying and products finishing. Comparing with the prior art, the invention provides a multiple usage method of the seeding watermelon, in particular to the peel, the dregs or the juice of the seeding watermelon. At the same time, with the invention, large raw material resource for the pectin production is found and the resource is utilized fully, thereby having a great economic prospect.
Description
Technical field:
The present invention relates to the method for comprehensive utilization of an a kind of kind of watermelon, the method for comprehensive utilization of especially a kind of kind of watermelon skin, scum juice and the method for from a kind of watermelon, extracting pectin, special one is kind of a method of from kind of watermelon skin scum juice, extracting pectin.
Background technology:
A kind of watermelon is claimed the seed melon again, and all there is cultivation especially northern various places in China various places, and the major production areas is the provinces and regions, northwest, is very important industrial crops, accounts for first of the whole nation and has realized large-scale planting like the Xinjiang cultivated area.
And a present kind of watermelon mainly is to get seed; Getting skin behind the seed, slag etc. has only few part to be utilized to the feed as livestock; Because it is difficult to long term storage, so the overwhelming majority all is dropped a large amount of melon juice that produce when especially getting seed, flesh etc.; Then be dropped fully, caused a large amount of wastes of resource.
Therefore, a kind ofly a kind of watermelon is got the comprehensive utilization that residue behind the seed such as skin slag wait until just seem very necessary.
A kind of watermelon belongs to Curcurbitaceae, according to " book on Chinese herbal medicine is sended relief to a famine area " record, " seed melon nature and flavor are sweet, relieving summer-heat, cough-relieving arranged, promote the production of body fluid, diuresis, moistening lung, quench the thirst, aid digestion effect, abdomen work gathers, eliminates and bursts swollenly in can curing, fitting is stomach medicine for oral administration ".Prove that through the people long-term practice except that above effect, the seed melon has more and relieves inflammation or internal heat, relieving alcoholism, protects the liver dirty and treat illnesss such as chronic stomach cold disease, dysentery, hypertension, silicosis, pneumoconiosis.Seed melon juice has more special effective function to skin maintenance, its low sugar, low fat, low in calories, diabetes patient's health-care good product especially.
Find that after deliberation kind of watermelon melon pulp, melon skin and melon juice also are rich in pectin, are the desirable pectin resources of production; According to surveying and determination; The pectin content of its melon juice, melon skin is more than 0.5%, and then about 12%, the gained dry is again extraordinary feed to dried melon skin behind the extraction pectin.
Pectin (Pectin) is a kind of polysaccharose substance of separation and Extraction from plant tissue; Come from apple and oranges and tangerines; It is a kind of water-soluble dietary fiber of green natural; The world in 1981 joins agricultural tissue-estimating, and it is the food additives that do not have intake restriction every day (ADI-value), because its significant gelatification has ten minutes purposes widely in the modern industrial; In food industry, it is to make indispensable stabilizing agents such as jam, jelly, sour milk, candy, ice cream, fruit beverage; In medical industry, can be used for preparing laxative, styptic, toxic metal antidote and blood substitutes etc., the pharmacological action that also can be used to prolong antibiotic; In textile industry, can be used for replacing starch and need not other assistant; In wood-processing industry, be good adhesive; Also can be used to make cosmetics in the production in light industry and alternative agar is made the culture medium of certain micro-organisms, and can be used as the emulsifying agent between oil and the water.Pectin is divided into two kinds of high ester, low esters, and the latter is divided into low ester of tradition and the low ester gum of amidatioon.In functional food, have good gel, thickening, stable and emulsification respectively according to its characteristic.Pectin is plant polyose, is a kind of dietary fiber, and its health-care effect is except reducing plasma cholesterol, regulate blood sugar level, the prevention of obesity, can also suppressing the formation of cancer cell diffusion or tumour.
At present; Has only seldom several Europe and U.S.'s manufacturer production pectin in the world; Like the CPKELCO company of Denmark and DENISCO company, German H&F company, the OBIPEKTINAG company of Switzerland and the CARGILL company of the U.S., the production and sales of pectin are monopolized by offshore company.
In recent years, the domestic and international market demand increases day by day, and the volume of world trade of pectin is about about 36,000 tons, and annual with the 5%--6% speed increase, and the international market price of pectin is about 1.25 ten thousand dollars/ton, because the pectin demand is far longer than supply.Therefore, the prospect of production of pectin is very good.Domestic annual requirement is about 2000 tons, and supply falls short of demand and cost an arm and a leg.Because of be correlated with dairy products and beverage output year increase 40～50%, the demand of pectin is also increased thereupon.
Existing pectin is obtained approach, has only few in number several kinds, knownly can extract raw material at the pectin of commercial Application and mainly contain oranges and tangerines and skin, sunflower plate and bar, apple, beet and slag, flax, shaddock, lemon, potato etc.Therefore in the pectin production process, not only receive the restriction of raw material scale, also be limited by cost of material, material quality and obtain the restriction of pectin technical conditions.Thereby at present domesticly have only seldom several manufacturer production pectin, and all because of the deficiency of raw materials for production, production scale is restricted.
Like disclosed method and the disclosed method of utilizing pericarp to produce pectin of CN101011117 of from the citrus pericarp, extracting pectin of Chinese patent CN1923853; Mainly utilize pericarp production pectin such as oranges and tangerines skin, its technical process comprises following steps: the pericarp fragment is soaked the back remove juice with filter press under 60 ℃～90 ℃ temperature; Acid is carried: in the water of PH 1.5～4.5,70 ℃～95 ℃ following acid of water temperature are carried with pomace; Concentrate: get filtrating with filter press and concentrate; Alcohol extracting: precipitate with adding ethanol in the concentrate; Press filtration: filter with filter press, filter cake is pulverized obtained pectin again.
The disclosed extracting pectin of Chinese patent CN101037485 then is from the mixture of pumpkin pulp and pumpkin peel, to extract pectin, the production method of the disclosed pectin of CN1310186, and its raw material is oranges and tangerines skin, sunflower plate and bar, megasse; CN1703429 discloses the method that a kind of processing contains the vegetable material of pectin; Its related material that contains pectin comprises cedra fruits, other fruit such as apple, beet; Residue during soybean protein is produced; Linseed or flax, aloe, sunflower bud etc.
Because preparation, processing in different material are far from each other on technology; Directly have influence on result thereafter; And a kind of watermelon; Particularly get the characteristics that skin, the juice flesh of the kind of watermelon behind the seed have not anti-storage, very easily rot, thereby correctly carry out preliminary treatment and just become vital problem getting kind of watermelon skin, juice flesh behind the seed.
Summary of the invention:
The purpose of this invention is to provide an a kind of kind of watermelon, the especially method of comprehensive utilization of kind of watermelon skin, slag or juice, another object of the present invention then provides a kind of method of from a kind of watermelon, extracting pectin of the method for comprehensive utilization according to an above-mentioned kind of watermelon or its skin, scum juice.
The method of comprehensive utilization of a kind of watermelon of the present invention is characterized in from a kind of watermelon, extracting pectin with a kind of watermelon as raw material.
The method of comprehensive utilization of an above-mentioned kind of watermelon, the said pectin that from a kind of watermelon, extracts is meant especially skin or the juice flesh after a kind of watermelon is got seed and extracts pectin.
The method of from a kind of watermelon, extracting pectin of the present invention, mainly form by following technical process:
Raw material collection, preliminary treatment, acid are carried, filter, are concentrated, alcohol extracting, drying, finished product, and its characteristics are that described raw material is collected as: a ripe kind of watermelon is removed seed, collect remaining kind of watermelon mixture;
Said preliminary treatment is: subsequent use to the fresh kind of watermelon mixture pulverizing and the enzyme processing postprecipitation that goes out.
Get into acid afterwards and put forward program.
As further preferred version
Described kind of watermelon mixture is the mixture of kind of watermelon flesh, juice,
The said enzyme that goes out is: add 0.1～0.3% salt by weight, be warmed to 50～95 ℃, the horizontal high voltage impulse electric field of going forward side by side is handled; Its static electric field is 100～1000V/cm, electric field treatment intensity 30～100KV/cm, pulse width 1～100 microsecond; Frequency 1～30KHz, 2～100 of umber of pulses.
As another technical scheme of the present invention
Described kind of watermelon mixture is a kind of watermelon skin;
The said enzyme that goes out is: place more than 95 ℃ and distilled under the temperature 5～12 minutes, having water logging to go out with surperficial shrinkage is benefit, with the passivation pectinase activity, gets into acid afterwards and puies forward program.
The said enzyme that goes out also can be: a. places more than 95 ℃ temperature to distill 5～12 minutes kind of watermelon skin, dehydrates to water content≤15% subsequent use then; B. kind of watermelon skin is done further and pulverized, make its particle, insert in the container less than below the 5mm; Add 10～25 times of water by weight; 20～50 ℃ of water temperatures also transfer to pH 5.5～6.3 subaciditys, add 0.5～1.5% calgon by weight, soak after 60-120 minute to get into acid and put forward program.
The said enzyme that goes out also can be: a. with kind of watermelon skin in temperature below 45 ℃, be acidifying water washing 5-12 minute of 3-4 with the pH value, with the passivation pectinase activity, dehydrate to water content≤15% subsequent use then; B. kind of watermelon skin is done further and pulverized, make its particle, insert in the container less than below the 5mm; Add 10～25 times of water by weight; 20～50 ℃ of water temperatures also transfer to pH 5.5～6.3 subaciditys, add 0.5～1.5% calgon by weight, soak after 60-120 minute to get into acid and put forward program.
As further improvement project; Above-mentioned acid is carried and being preferably: above-mentioned pretreated mixed liquor is transferred to pH=1～4 with acid, and heated and stirred is also filtered at any time and is collected the pectin extract, measures at any time simultaneously and continue to add the acid adjusting to keep the pH value between 1～4; When being heated to 55～95 ℃, stop to add acid; Keep the said temperature scope, do not stop to stir 50～70 minutes, cross with 120～250 μ m sieve or filter cloth and filter the pectin extract.
As preferred scheme, above-mentionedly continue to add during acid regulates, its acidity value preferably is to grow from weak to strong and carries out level time adjusting.
As preferred scheme, preferably use stainless steel, aluminium, one type of non iron container of plastics in above-mentioned each operation.
As further improvement, the shape of above-mentioned kind of watermelon skin chopping preferably is sheet type melon silk, 2～5 millimeters of silk thickness.
Above-mentioned acid will be decoloured after carrying; Can adopt the sulphur method of floating to discolor; Or by the processing of decolouring with sodium sulfite or sodium hydrogensulfite, also available following method: in filtrating, add 0.3～0.5% active carbon by weight, 55～80 ℃ down decolouring after 20～30 minutes with the industrial filter cloth press filtrations of≤60 μ m; Stir the back with 1%～3% diatomite again and under 65～90 ℃ of temperature, keep using again in 20 ~ 30 minutes≤the industrial filter cloth press filtration of 60 μ m, collect filtrating; Also available other existing decoloration process.
Described concentrating can be following method: the pectin extract of acid being carried gained is used the vacuum concentration method under 55～85 ℃ condition, pectin is concentrated into solid content >=5%;
Described alcohol extracting can be the alcohol that in fructose concentrating liquid, adds weight 100%-200% concentration 90%-95% by weight; The limit edged stirs; The pectin deposition is separated out, centrifugal under 4000-8000 rev/min rotating speed, filter, remove alcohol dissolubility impurity with≤60 μ m sieve;
Dry: the pectin of alcohol extracting is sent into vacuum drier 1-2 hour or is placed baking box below 75 ℃, be dried to water content below 10%, pulverized 150-250 μ m sieve to pectin, obtain pectin powder, pack the jelly powder finished product.
Compared with prior art, the invention provides an a kind of kind of watermelon, the especially method of comprehensive utilization of kind of watermelon skin, slag or juice, also found a kind of very large raw material sources simultaneously, utilized resource fully, very large economic utilization prospect is arranged for pectin production.
The specific embodiment:
Embodiment 1:
Get maturation and remove seed and the kind of watermelon flesh of skin, the mixture of juice, melon pulp is crushed to the particle below the 5mm, contains in the rustless steel container; The salt of adding 0.1% is warmed to 85 ℃, uses the high-pressure pulse electric treatment facility again; Static electric field is 300V/cm, with electric field treatment intensity 90KV/cm, and pulse width 90 microseconds; Frequency 12KHz, 90 of umber of pulses are to the kind of watermelon liquid enzyme that goes out.In kind of watermelon juice, add hydrochloric acid and transfer pH to 2.5, evenly be heated to 85 ℃, in fully stirring, kept constant temperature 30 minutes; Cross the squeezing of 210 μ m plate and frame filter press afterwards, must filtrate, add 0.3% active carbon; Decoloured 30 minutes down at 65 ℃, after 20 minutes, filter with 48 μ m filter clothes; Under 85 ℃ of temperature conditions, again filtrating is concentrated, be concentrated into pectin content to 6% after, be cooled to below 45 ℃.Twice adding concentration is that 94% alcohol makes the pectin deposition by weight in concentrate, filters with filter press, and the pectin that leaches is sent in 70 ℃ of baking boxs, is dried to water content 5%; Pectin is pulverized, behind the 150 μ m sieve, obtained white and have a little lurid pectin powder excessively.The filtrating recovered alcohol recycles.
Embodiment 2:
Get maturation and remove seed and the kind of watermelon flesh of skin, the mixture of juice, melon pulp is crushed to the particle below the 3mm, contains in the rustless steel container; Add 0.3% salt by weight, be warmed to 75 ℃, the horizontal high voltage impulse electric field of going forward side by side is handled; Its static electric field is 500V/cm, electric field treatment intensity 80KY/cm, pulse width 80 microseconds; Frequency 5KHz, 40 of umber of pulses are to the kind of watermelon liquid enzyme that goes out.In kind of watermelon juice, add hydrochloric acid when temperature is reduced to 45 ℃ and transfer pH to 2.8, evenly heat and stirs, the every rising of temperature is afterwards tested for 10 ℃ and is also regulated one time acid number 0.2; Promptly the pH value is adjusted to 2.6 50 ℃ the time; The pH value was adjusted to 2.0 when the pH value was adjusted to 2.2,80 ℃ when the pH value was adjusted to 2.4,70 ℃ in the time of 60 ℃; Stop to add acid afterwards, remain on 90 ℃ during to 90 ℃ and do not stop to stir 45 minutes.The gained pectin solution is crossed the plate compression squeezing, must filtrate, after filtering with 250 μ m sieve, add 0.3% active carbon, decolouring is 30 minutes under 65 ℃, after 20 minutes, filters with 58 μ m filter clothes; Under 85 ℃ of temperature conditions, again filtrating is concentrated, be concentrated into pectin content to 6% after, be cooled to below 45 ℃.Twice adding concentration is that 94% alcohol makes the pectin deposition by weight in concentrate, filters with 58 μ m filter presses, and the pectin that leaches is sent in 70 ℃ of baking boxs, is dried to water content 5%; Pectin is pulverized, behind the 210 μ m sieve, obtained white and have a little lurid pectin powder excessively.The filtrating recovered alcohol recycles.
Embodiment 3:
With removing the seed and the kind of watermelon flesh of skin, the mixture of juice, contain in the resistant to elevated temperatures plastic containers, add 0.15% salt, be warmed to 95 ℃; The horizontal high voltage impulse electric field of going forward side by side is handled, and static electric field is 400V/cm, electric field treatment intensity 60KV/cm; Pulse width 5 microseconds, frequency 20KHz, 80 of umber of pulses; The kind of watermelon liquid enzyme that goes out is handled postprecipitation and is cooled to 35 ℃, said mixed liquor is transferred to pH=3 with hydrochloric acid, heated and stirred; Measure at any time simultaneously and continue to add acid for adjusting pH value, every rising regulates 0.3 for 5 ℃, when pH value is 1.8 to stop adjusting; When continuing to be heated to 90 ℃, keep temperature not stop to stir filtering after 60 minutes collecting the pectin extract, discolor with the sulphur method of floating afterwards.Under 65 ℃ condition, use the vacuum concentration method, pectin is concentrated into solid content 10%, adding weight 200% concentration is 95% alcohol in fructose concentrating liquid; The limit edged stirs, and the pectin deposition is separated out, and 60 μ m sieve is centrifugal under 8000 rev/mins rotating speed; Remove alcohol dissolubility impurity, the pectin of alcohol extracting is sent into vacuum drier be dried to water content 5%, pulverized 250 μ m sieve; Obtain pectin powder, pack the jelly powder finished product.
Embodiment 4:
Get maturation and remove seed and the kind of watermelon flesh of skin, the mixture of juice, melon pulp is crushed to the particle below the 3mm, contains in the rustless steel container; The salt of adding 0.18% is warmed to 95 ℃, uses the high-pressure pulse electric treatment facility; Static electric field is 100V/cm, electric field treatment intensity 50KY/cm, pulse width 100 microseconds; Frequency 10KHz, 50 of umber of pulses are to the kind of watermelon liquid enzyme that goes out.In kind of watermelon juice, add hydrochloric acid when temperature is reduced to 45 ℃ and transfer pH to 2.8, evenly heating, 10 ℃ of tests of the every rising of temperature are afterwards also regulated acid number 0.2 one time; Promptly the pH value is adjusted to 2.6 50 ℃ the time; The pH value was adjusted to 2.0 when the pH value was adjusted to 2.2,80 ℃ when the pH value was adjusted to 2.4,70 ℃ in the time of 60 ℃; Stop to add acid afterwards, remain on 90 ℃ during to 90 ℃ and do not stop to stir 45 minutes.The gained pectin solution is crossed the plate compression squeezing, must filtrate.After leachate filters with 210 μ m sieve, add 0.3% active carbon, decoloured 30 minutes down, after 20 minutes, filter with filter cloth at 65 ℃; Under 85 ℃ of temperature conditions, again filtrating is concentrated, be concentrated into pectin content to 6% after, be cooled to below 45 ℃.Twice adding concentration is that 94% alcohol makes the pectin deposition by weight in concentrate, filters with 60 μ m filter presses, and the pectin that leaches is sent in 70 ℃ of baking boxs, is dried to water content 5%; Pectin is pulverized, behind the 150 μ m sieve, obtained white and have a little lurid pectin powder excessively.Reclaim the alcohol in the filtrating, recycle.
Embodiment 5:
Get maturation and remove seed and the kind of watermelon flesh of skin, the mixture of juice, melon pulp is crushed to the particle below the 4mm, contains in the rustless steel container; Add 0.25% salt by weight, be warmed to 95 ℃, the horizontal high voltage impulse electric field of going forward side by side is handled; Its static electric field is 200V/cm, electric field treatment intensity 70KV/cm, pulse width 60 microseconds; Frequency 18KHz, 10 of umber of pulses, enzyme goes out.In kind of watermelon juice, add hydrochloric acid when temperature is reduced to 45 ℃ and transfer pH to 2.8, evenly heating, 10 ℃ of tests of the every rising of temperature are afterwards also regulated acid number 0.2 one time; Promptly the pH value is adjusted to 2.6 50 ℃ the time; The pH value was adjusted to 2.0 when the pH value was adjusted to 2.2,80 ℃ when the pH value was adjusted to 2.4,70 ℃ in the time of 60 ℃; Stop to add acid afterwards, remain on 90 ℃ during to 90 ℃ and do not stop to stir after 45 minutes to filter and collect the pectin extract.The gained pectin solution is crossed the squeezing of 210 μ m plate compressions, must filtrate, add 0.3% active carbon, decoloured 30 minutes down, after 20 minutes, filter with 38 μ m filter clothes at 65 ℃; Under 85 ℃ of temperature conditions, again filtrating is concentrated, be concentrated into pectin content to 6% after, be cooled to below 45 ℃.Twice adding concentration is that 94% alcohol makes the pectin deposition by weight in concentrate, filters with 38 μ m filter presses, and the pectin that leaches is sent in 70 ℃ of baking boxs, is dried to water content 5%; Pectin is pulverized, behind the 180 μ m sieve, obtained white and have a little lurid pectin powder excessively.The filtrating recovered alcohol recycles.
Embodiment 6:
The kind of watermelon of maturation is removed seed and skin, collect the mixture of melon pulp, juice, contain in the rustless steel container, add 0.2% salt; Be warmed to 50 ℃, the horizontal high voltage impulse electric field of going forward side by side is handled, and its static electric field is 800V/cm, electric field treatment intensity 30KV/cm; Pulse width 40 microseconds, frequency 30KHz, 100 of umber of pulses are handled postprecipitation and are cooled to 40 ℃ the kind of watermelon liquid enzyme that goes out; Transfer to pH=3 with citric acid, continue heated and stirred, the while is measured at any time and continues to add acid for adjusting pH value, and acid number 0.2 is also regulated one time in 5 ℃ of tests of the every rising of temperature; The pH value was adjusted to 2.2 when the pH value was adjusted to 2.4,60 ℃ when the pH value was adjusted to 2.6,55 ℃ when promptly the pH value was adjusted to 2.8,50 ℃ 45 ℃ the time; The pH value is adjusted to 2.0 in the time of 65 ℃, stops to add acid afterwards, continues heating and maintains the temperature at 90 ℃ and do not stop to stir to filter after 50 minutes and collect the pectin extract; The active carbon of adding 0.5% in filtrating, after decolouring 30 minutes under 60 ℃, the industrial filter cloth press filtration of 25 μ m; Stir the back with 2% diatomite again and under 90 ℃ of temperature, kept 20 minutes, use the industrial filter cloth press filtration of 25 μ m again, collect filtrating; Acid is carried the pectin extract of gained and under 80 ℃ condition, used the vacuum concentration method, pectin is concentrated into solid content 12%, adding weight 150% concentration is 90% alcohol; The limit edged stirs, and the pectin deposition is separated out, and is centrifugal at 5000 rev/mins rotating speeds, 38 μ m sieve; Remove and send into vacuum drier behind the alcohol dissolubility impurity and be dried to water content 6%; Pulverized 210 μ m sieve, obtained pectin powder, pack the jelly powder finished product.
Embodiment 7:
Get maturation and remove seed and the kind of watermelon flesh of skin, the mixture of juice, melon pulp is crushed to the particle below the 2mm, contains in the rustless steel container, adds 0.3% salt, be warmed to 95 ℃ 15 minutes, enzyme goes out.In kind of watermelon juice, add hydrochloric acid and transfer pH to 2.0, evenly be heated to 70 ℃, in fully stirring, kept constant temperature 40 minutes; And filter at any time and collect the pectin extract; Cross 210 μ m sieve plate frame press filtrations squeezing, must filtrate, add 0.3% active carbon; Decoloured 30 minutes down at 65 ℃, after 20 minutes, filter with 50 μ m sieving cloth; Under 85 ℃ of temperature conditions, again filtrating is concentrated, be concentrated into pectin content to 6% after, be cooled to below 45 ℃.Twice adding concentration is that 94% alcohol makes the pectin deposition by weight in concentrate, filters with 50 μ m sieve filter press, and the pectin that leaches is sent in 70 ℃ of baking boxs, is dried to water content 5%; Pectin is pulverized, behind the 210 μ m sieve, obtained white and have a little lurid pectin powder excessively.The filtrating recovered alcohol recycles.
Embodiment 8:
Get fresh kind of watermelon skin and cut the 5mm silk, put into 105 ℃ in steamer and steamed 12 minutes down, add the water of 2 times of weight, when 40 ℃ of left and right sides of mixed liquor with salt acid for adjusting pH value to 4; The beginning heated and stirred, every intensification is simultaneously measured a pH value for 10 ℃, and pH value increase by 0.4 when at every turn regulating; The pH value was adjusted to 2.8 when the pH value was adjusted to 3.2,70 ℃ when promptly the pH value was adjusted to 3.6,60 ℃ 50 ℃ the time; The pH value was adjusted to 2.0 when the pH value was adjusted to 2.4,90 ℃ in the time of 80 ℃, stopped to add acid afterwards; Keep temperature not stop for 90 ℃ to stir filtering after 50 minutes collecting the pectin extract, the gained pectin solution is carried in acid under 55 ℃ condition, used the vacuum concentration method, pectin is concentrated into solid content 7% with the sulphur method of the floating back of discoloring; 1.5 times of concentration of adding fructose concentrating liquid weight are 95% alcohol, and the limit edged stirs, and the pectin deposition is separated out; Centrifugal at 6000 rev/mins rotating speeds, 60 μ m sieve, remove alcohol dissolubility impurity, pectin after the alcohol extracting is sent into vacuum drier under 65 ℃, be dried to water content 10%; Pulverized 150 μ m sieve to pectin, obtained pectin powder, pack the jelly powder finished product.
Embodiment 9:
Get fresh kind of watermelon skin and cut the 3mm silk, put into 110 ℃ in steamer and steamed 12 minutes down, add the water of 1.5 times of weight, when 35 ℃ of mixed liquors with salt acid for adjusting pH value to 3; The every intensification simultaneously of beginning heated and stirred is measured a pH value for 10 ℃, and pH value 0.4 when at every turn regulating, and promptly the pH value is adjusted to 2.6 50 ℃ the time; The pH value was adjusted to 1.8 when the pH value was adjusted to 2.2,70 ℃ in the time of 60 ℃, stopped to add acid afterwards; Continue heating and keep temperature not stop for 90 ℃ to stir filtering after 50 minutes collecting the pectin extract, the gained pectin solution is carried in acid under 65 ℃ condition, used the vacuum concentration method, pectin is concentrated into solid content 7% with the sulphur method of the floating back of discoloring; 1.5 times of concentration of adding fructose concentrating liquid weight are 95% alcohol, and the limit edged stirs, and the pectin deposition is separated out; Centrifugal at 6000 rev/mins rotating speeds, 40 μ m sieve, remove alcohol dissolubility impurity, pectin after the alcohol extracting is sent into vacuum drier under 65 ℃, be dried to water content 10%; Pulverized 150 μ m sieve to pectin, obtained pectin powder, pack the jelly powder finished product.
Embodiment 10:
Get the strip that is cut into width 50mm after the fresh kind of watermelon severe edema due to hypofunction of the spleen is washed, using pH value is that 3.5 acidifying water washed 10 minutes kind of watermelon silk, dries to water content≤15% subsequent use then.Above-mentioned kind of watermelon skin dry grinding of drying to particle 4mm, is put into 15 times of water of weight, add 1% calgon, soaked 60 minutes.Use salt acid for adjusting pH value to 2 then, heat temperature raising to 95 ℃ after fully stirring 100 minutes under this temperature conditions, with the filtration of 200 μ m sieve, must be filtrated.The active carbon of adding 0.5% in filtrating; Decoloured 30 minutes down at 70 ℃; The industrial filter cloth press filtration of 50 μ m, 2% diatomite stir the back and under 80 ℃ of temperature, kept 30 minutes, use the industrial filter cloth press filtration of 50 μ m again; Gained filtrating is used the vacuum concentration method under 70 ℃ condition, pectin is concentrated into solid content 8%; In fructose concentrating liquid, add the alcohol of 1.5 times of weight, concentration 90%, the limit edged stirs, and is centrifugal under 6500 rev/mins rotating speeds, 40 μ m sieve after the pectin deposition is separated out, and removes alcohol dissolubility impurity; Pectin after the alcohol extracting is sent in 70 ℃ of following baking boxs, is dried to water content below 8%, pulverized 200 μ m sieve, obtain pectin powder, pack the jelly powder finished product.
Embodiment 11:
Fresh kind of watermelon skin and the washing behind the seed got in collection, is cut into the 40mm piece, under 35 ℃, is 3 acidifying water washing 6 minute with the pH value in temperature, and it is 15% subsequent use sending into then that dryer dehydrates under 90 ℃ to water content.
Kind of watermelon skin is done further pulverizing, and making its particle is 3mm, inserts in the rustless steel container; Add 20 times of water,, add 1% calgon in 50 ℃ of subaciditys of descending and transferring to pH=6 of water temperature; Soak and transfer to pH=2.5 with hydrochloric acid after 60 minutes, begin heating afterwards, when being heated to 85 ℃ and keep said temperature not stop to stir filtering after 70 minutes collecting the pectin extract; With the sulphur method of floating discolor the back under 80 ℃ temperature, use the vacuum concentration method, pectin is concentrated into solid content >=9%; Adding weight 200% concentration is 95% alcohol in fructose concentrating liquid; The limit edged stirs; It is centrifugal at 7500 rev/mins rotating speed 38 μ m sieve that pectin deposition is separated out the back, removes to send into vacuum drier behind the alcohol dissolubility impurity and be dried to water content 8%, pulverized 180 μ m sieve; Obtain pectin powder, pack the jelly powder finished product.
Embodiment 12:
Fresh kind of watermelon skin and the washing behind the seed got in collection, and the piece that is cut into 60mm distilled 5 minutes in 120 ℃ of temperature, and it is 12% subsequent use using vacuum drier under 80 ℃, to dehydrate to water content then.
Kind of watermelon skin is done further pulverizing, and making its particle is 2mm, inserts in the rustless steel container, adds 25 times of water; 40 ℃ of water temperatures also transfer to pH 5.5 subaciditys, soak after 120 minutes to begin heating after transferring to pH=4 with hydrochloric acid, and acid number 0.2 is also regulated one time in 5 ℃ of tests of the every rising of temperature, and promptly the pH value is adjusted to 3.8 45 ℃ the time; The pH value was adjusted to 3.0 when the pH value was adjusted to 3.2,65 ℃ when the pH value was adjusted to 3.4,60 ℃ when the pH value was adjusted to 3.6,55 ℃ in the time of 50 ℃; The pH value was adjusted to 2.2 when the pH value was adjusted to 2.4,85 ℃ when the pH value was adjusted to 2.6,80 ℃ when the pH value was adjusted to 2.8,75 ℃ in the time of 70 ℃; The pH value is adjusted to 2.0 in the time of 90 ℃, stops to add acid afterwards, remains on 90 ℃ and does not stop to stir after 60 minutes to filter and collect the pectin extract, discolors with the sulphur method of floating; Use the vacuum concentration method down at 75 ℃ then, it is 6% that pectin is concentrated into solid content, and adding weight 100% concentration is 92% alcohol, and the limit edged stirs; The pectin deposition is separated out, and the centrifugal alcohol dissolubility impurity of removing of 48 μ m sieve is sent into the pectin after the alcohol extracting in 70 ℃ of baking boxs under 6000 rev/mins rotating speed, is dried to water content 9%; Pulverized 180 μ m sieve, obtained pectin powder, pack the jelly powder finished product.
Embodiment 13:
After a kind of watermelon is got seed, collect fresh kind of watermelon skin and washing by peasant household, the bar or the piece that are cut into 50mm distilled 7 minutes in 110 ℃ of temperature, and to dehydrate to water content be 15% subsequent use in Exposure to Sunlight then.
The kind of watermelon skin at peasant household place is done concentrated back further pulverize, making its particle is 4mm, inserts in the rustless steel container, adds 25 times of water; 45 ℃ of water temperatures also transfer to pH 5.6 subaciditys, soak to transfer to pH=3.6 with hydrochloric acid after 90 minutes, begin even heating afterwards, and 5 ℃ of tests of the every rising of temperature are also regulated acid number 0.2 one time; The pH value was adjusted to 2.8 when the pH value was adjusted to 3.0,65 ℃ when the pH value was adjusted to 3.2,60 ℃ when promptly the pH value was adjusted to 3.4,55 ℃ 50 ℃ the time; The pH value was adjusted to 2.0 when the pH value was adjusted to 2.2,85 ℃ when the pH value was adjusted to 2.4,80 ℃ when the pH value was adjusted to 2.6,75 ℃ in the time of 70 ℃; The pH value is adjusted to 1.8 in the time of 90 ℃, stops to add acid afterwards, remains on 90 ℃ and does not stop to stir after 60 minutes to filter and collect the pectin extract, discolors with the sulphur method of floating; Use the vacuum concentration method down at 75 ℃ then, it is 10% that pectin is concentrated into solid content, and adding weight 180% concentration is 95% alcohol, and the limit edged stirs; The pectin deposition is separated out, and the centrifugal alcohol dissolubility impurity of removing of 38 μ m sieve is sent into the pectin after the alcohol extracting in 70 ℃ of vacuum driers under 5000 rev/mins rotating speed, is dried to water content 9%; Pulverized 220 μ m sieve, obtained pectin powder, pack the jelly powder finished product.
Embodiment 14:
After a kind of watermelon is got seed, collect fresh kind of watermelon skin and washing by peasant household, bar or the piece that is cut into 30mm is that 3.5 acidifying water washed 10 minutes at 25 ℃, pH value, and to dehydrate to water content be 13% subsequent use in Exposure to Sunlight then.
The kind of watermelon skin at peasant household place is done concentrated back further pulverize, making its particle is 3mm, inserts in the rustless steel container, adds 15 times of water; 40 ℃ of water temperatures also transfer to pH 5.8 subaciditys, add 0.4% calgon, soak to transfer to pH=3.5 with hydrochloric acid after 80 minutes, begin heating afterwards; Acid number 0.3 is also regulated one time in 10 ℃ of every risings of temperature test, and the pH value was adjusted to 2.6 when the pH value was adjusted to 2.9,70 ℃ when promptly the pH value was adjusted to 3.2,60 ℃ 50 ℃ the time; The pH value was adjusted to 2.0 when the pH value was adjusted to 2.3,90 ℃ in the time of 80 ℃, stopped to add acid afterwards, remained on 90 ℃ and did not stop to stir after 55 minutes to filter and collect the pectin extract; Discolor with the sulphur method of floating, use the vacuum concentration method down at 75 ℃ then, it is 10% that pectin is concentrated into solid content; Adding weight 150% concentration is 95% alcohol, and the limit edged stirs, and the pectin deposition is separated out; The centrifugal alcohol dissolubility impurity of removing of 45 μ m sieve is sent into the pectin after the alcohol extracting in 65 ℃ of vacuum driers under 8000 rev/mins rotating speed, is dried to water content 7%; Pulverized 250 μ m sieve, obtained pectin powder, pack the jelly powder finished product.
Embodiment 15:
After a kind of watermelon is got seed, collect fresh kind of watermelon skin and washing by peasant household, bar or the piece that is cut into 25mm is that 4 acidifying water washed 10 minutes at 20 ℃, pH value, and to dehydrate to water content be 14% subsequent use in Exposure to Sunlight then.
The kind of watermelon skin at peasant household place is done concentrated back further pulverize, making its particle is 2mm, inserts in the rustless steel container, adds 10 times of water; 35 ℃ of water temperatures also transfer to pH 6.2 subaciditys, add 0.6% calgon, soak to transfer to pH=3.6 with sulfuric acid after 60 minutes, begin heating afterwards; Acid number 0.3 is also regulated one time in 10 ℃ of every risings of temperature test, and the pH value was adjusted to 2.7 when the pH value was adjusted to 3.0,70 ℃ when promptly the pH value was adjusted to 3.3,60 ℃ 50 ℃ the time; The pH value was adjusted to 2.1 when the pH value was adjusted to 2.4,90 ℃ in the time of 80 ℃, stopped to add acid afterwards, remained on 90 ℃ and did not stop to stir after 55 minutes to filter and collect the pectin extract; Discolor with the sulphur method of floating, use the vacuum concentration method down at 75 ℃ then, it is 10% that pectin is concentrated into solid content; Adding weight 150% concentration is 95% alcohol, and the limit edged stirs, and the pectin deposition is separated out; The centrifugal alcohol dissolubility impurity of removing of 45 μ m sieve is sent into the pectin after the alcohol extracting in 65 ℃ of vacuum driers under 7000 rev/mins rotating speed, is dried to water content 7%; Pulverized 250 μ m sieve, obtained pectin powder, pack the jelly powder finished product.
Embodiment 16:
After a kind of watermelon is got seed, to collect fresh kind of watermelon skin and juice flesh respectively, and be cut into the silk of 3mm after the severe edema due to hypofunction of the spleen washed, melon pulp is crushed to less than 5mm; To mix skin silk, juice, flesh then and be mixed and heated to 95 ℃ of 10 minutes enzymes that go out, and be cooled to and add acid under 45 ℃ and transfer to pH=3.5, and begin heating afterwards, acid number 0.3 is also regulated one time in 10 ℃ of tests of the every rising of temperature; The pH value was adjusted to 2.3 when the pH value was adjusted to 2.6,80 ℃ when the pH value was adjusted to 2.9,70 ℃ when promptly the pH value was adjusted to 3.2,60 ℃ 50 ℃ the time; The pH value is adjusted to 2.0 in the time of 90 ℃, stops to add acid afterwards, remains on 90 ℃ and does not stop to stir after 40 minutes to filter and collect the pectin extract; Discolor with the sulphur method of floating, use the vacuum concentration method down at 75 ℃ then, it is 10% that pectin is concentrated into solid content; Adding weight 180% concentration is 95% alcohol, and the limit edged stirs, and the pectin deposition is separated out; The centrifugal alcohol dissolubility impurity of removing of 38 μ m sieve is sent into the pectin after the alcohol extracting in 65 ℃ of vacuum driers under 7000 rev/mins rotating speed, is dried to water content 7%; Pulverized 210 μ m sieve, obtained pectin powder, pack the jelly powder finished product.
Embodiment 17:
After a kind of watermelon is got seed, collect fresh kind of watermelon skin and juice flesh respectively, and be cut into the silk of 4mm after the severe edema due to hypofunction of the spleen washed, the kind of watermelon silk enzyme that goes out; With kind of watermelon liquid heat to 90 ℃, the horizontal high voltage impulse electric field of going forward side by side is handled again, and static electric field is 800V/cm, electric field treatment intensity 75KV/cm; Pulse width 15 microseconds, frequency 12KHz, 70 of umber of pulses are handled the kind of watermelon liquid enzyme that goes out; Silk, juice, flesh mix, and extraordinarily go into melon juice by 3 of melon silk amount, add 0.15% salt again, transfer to pH=3.3 with hydrochloric acid; Begin heated and stirred afterwards, measure at any time simultaneously and continue to add acid for adjusting pH value, every rising regulates 0.3 for 5 ℃, when pH value is 1.8 to stop adjusting; When continuing to be heated to 90 ℃, keep temperature not stop to stir filtering after 65 minutes collecting the pectin extract, discolor with the sulphur method of floating afterwards.Under 65 ℃ condition, use the vacuum concentration method, pectin is concentrated into solid content 5%, adding weight 130% concentration is 95% alcohol in fructose concentrating liquid; The limit edged stirs, and the pectin deposition is separated out, and 35 μ m sieve is centrifugal under 5500 rev/mins rotating speed; Remove alcohol dissolubility impurity, the pectin of alcohol extracting is sent into vacuum drier be dried to water content 7%, pulverized 250 μ m sieve; Obtain pectin powder, pack the jelly powder finished product.
Claims (3)
1. method of from a kind of watermelon, extracting pectin, mainly form by following technical process:
Raw material collection, preliminary treatment, acid are carried, filter, are concentrated, alcohol extracting, drying, finished product, it is characterized in that:
Described raw material is collected as: a ripe kind of watermelon is removed seed, collect remaining kind of watermelon mixture;
Said preliminary treatment is: fresh kind of watermelon mixture is pulverized and the enzyme processing of going out;
When kind of watermelon mixture was the mixture of kind of watermelon flesh, juice, the enzyme that goes out was: add 0.1～0.3% salt by weight, be warmed to 50～95 ℃; The horizontal high voltage impulse electric field of going forward side by side is handled; Its static electric field is 100～1000V/cm, electric field treatment intensity 30～100KV/cm, pulse width 1～100 microsecond; Frequency 1～30KHz, 2～100 of umber of pulses;
When kind of watermelon mixture is kind of watermelon skin; The enzyme that goes out is: a. places more than 95 ℃ temperature to distill 5～12 minutes kind of watermelon skin; Perhaps with kind of watermelon skin in temperature below 45 ℃, be acidifying water washing 5-12 minute of 3-4 with the pH value, dehydrate to Han Shui Liang ≦ 15% subsequent use then; B. kind of watermelon skin is done further and pulverized, make its particle less than 5mm, insert in the container, add 10～25 times of water by weight, 20～50 ℃ of water temperatures also transfer to pH 5.5～6.3 subaciditys, add 0.5～1.5% calgon by weight, soak 60-120 minute;
Described acid carry for: above-mentioned pretreated mixed liquor is transferred to pH=1～4 with acid; Heated and stirred is also filtered at any time and is collected the pectin extract; While is measured at any time and continues to add acid and regulate maintenance pH value between 1～4, when being heated to 55～95 ℃, stops to add acid, keeps this temperature range; Do not stop to stir 50～70 minutes, and crossed with 120～250 μ m sieve or filter cloth and filter the pectin extract;
Said simmer down to: the pectin extract of acid being carried gained is used the vacuum concentration method under 55～85 ℃ condition, pectin is concentrated into solid content Han Liang ≧ 5%;
Described alcohol extracting is: in fructose concentrating liquid, adding weight 100%-200% concentration by weight is the alcohol of 90%-95%; The limit edged stirs; The pectin deposition is separated out, and centrifugal ， Yong under 4000-8000 rev/min rotating speed ≦ 60 μ m sieve filters, removes alcohol dissolubility impurity;
Said drying is: the pectin of alcohol extracting is sent into vacuum drier 1-2 hour or is placed baking box below 75 ℃, be dried to water content below 10%, pulverized 150-250 μ m sieve to pectin, obtain pectin powder, pack the jelly powder finished product.
2. the method for from a kind of watermelon, extracting pectin according to claim 1 is characterized in that:
Saidly continue to add during acid regulates, its acidity value is to grow from weak to strong and carries out level time adjusting.
3. the method for from a kind of watermelon, extracting pectin according to claim 1 and 2, it is characterized in that: used container is stainless steel, aluminium, one type of non iron container of plastics in said each operation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101800574A CN101214031B (en) | 2007-12-29 | 2007-12-29 | Comprehensive utilization of seeding-watermelon and method for extracting pectin from seeding-watermelon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101800574A CN101214031B (en) | 2007-12-29 | 2007-12-29 | Comprehensive utilization of seeding-watermelon and method for extracting pectin from seeding-watermelon |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101214031A CN101214031A (en) | 2008-07-09 |
| CN101214031B true CN101214031B (en) | 2012-02-22 |
Family
ID=39620579
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007101800574A Expired - Fee Related CN101214031B (en) | 2007-12-29 | 2007-12-29 | Comprehensive utilization of seeding-watermelon and method for extracting pectin from seeding-watermelon |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101214031B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101919551A (en) * | 2010-05-24 | 2010-12-22 | 但建明 | The comprehensive utilization of seed watermelon wastes |
| CN103652714A (en) * | 2013-12-12 | 2014-03-26 | 甘肃靖远正生籽瓜科技有限公司 | Seed melon full-utilization processing production device and technology thereof |
| CN106722476A (en) * | 2016-12-12 | 2017-05-31 | 湖北工业大学 | Fat substitute and preparation method and application containing orange peel active component |
| CN106666519A (en) * | 2016-12-12 | 2017-05-17 | 湖北工业大学 | Fat substitute containing active ingredients of pomelo peel, as well as preparation method and application thereof |
| CN112899326A (en) * | 2021-03-31 | 2021-06-04 | 新疆大学 | Method for preparing melon peel pectin oligosaccharide with antibacterial activity by using immobilized enzyme |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1310186A (en) * | 2001-01-19 | 2001-08-29 | 华北工学院 | pectin producing method |
| CN1849943A (en) * | 2006-05-30 | 2006-10-25 | 殷涌光 | Method of sterilizing and enzyme-eliminating for fluid food |
| CN1923853A (en) * | 2005-09-01 | 2007-03-07 | 中南大学 | Extraction and preparation technology for pectin of orange pericarp |
| CN101011117A (en) * | 2006-07-06 | 2007-08-08 | 柴正荣 | Method for producing pectin utilizing peel |
| CN101037485A (en) * | 2007-04-20 | 2007-09-19 | 兰州大学 | Pectin extraction method |
-
2007
- 2007-12-29 CN CN2007101800574A patent/CN101214031B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1310186A (en) * | 2001-01-19 | 2001-08-29 | 华北工学院 | pectin producing method |
| CN1923853A (en) * | 2005-09-01 | 2007-03-07 | 中南大学 | Extraction and preparation technology for pectin of orange pericarp |
| CN1849943A (en) * | 2006-05-30 | 2006-10-25 | 殷涌光 | Method of sterilizing and enzyme-eliminating for fluid food |
| CN101011117A (en) * | 2006-07-06 | 2007-08-08 | 柴正荣 | Method for producing pectin utilizing peel |
| CN101037485A (en) * | 2007-04-20 | 2007-09-19 | 兰州大学 | Pectin extraction method |
Non-Patent Citations (1)
| Title |
|---|
| 万成志.西瓜皮提取果胶的生产技术.《应用科技》.1997,(第2期),11-12. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101214031A (en) | 2008-07-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104342337B (en) | A kind of production technique of Sunset Abelmoschus Root functional health wine | |
| CN101214031B (en) | Comprehensive utilization of seeding-watermelon and method for extracting pectin from seeding-watermelon | |
| CN102311906B (en) | Method for brewing active papaya wine | |
| CN101921686B (en) | Method for producing dry date wine | |
| CN101705151A (en) | Method for simultaneously extracting peanut oil and peanut albumen powder at low temperature | |
| CN105482957A (en) | Rhizoma polygonati extract, rhizoma polygonati wine thereof and rhizoma polygonati wine preparation method | |
| CN103478838A (en) | Honeysuckle kudzuvine root beverage and preparation method thereof | |
| CN104757564A (en) | Method for preparing dietary fibers by means of peanut shells | |
| CN106912964A (en) | Soluble dietary fiber and preparation method thereof | |
| CN104004592A (en) | Method for simultaneously extracting essential oil and pectin from fresh citrus peels | |
| CN105132249A (en) | Fermented plum wine making method | |
| CN103497861B (en) | A kind of making method of thick wine | |
| CN106190766A (en) | A kind of brewage process of Caulis et Folium Kochiae Hibiscus Sabdariffa Linn tea vinegar | |
| CN103908523A (en) | Method for extracting tea pigment from tea leaves and tea pigment soft capsule | |
| US10870612B1 (en) | Method for simultaneously extracting lycopene and citrulline from watermelon | |
| CN108823034A (en) | A kind of brewing method of honey raisin tree fruit wine | |
| CN109619581A (en) | A kind of tree peony salt and preparation method thereof | |
| CN102356882B (en) | Method utilizing brewer's grains to produce biological diet cellulose and product thereof | |
| CN102020723B (en) | Method for continuously extracting low-ester pectin and microcrystalline cellulose from jerusalem artichoke stalks | |
| CN111363619A (en) | Method for synchronously preparing peony seed cold-pressed oil and protein by enzyme method | |
| CN106008744A (en) | Method for preparing pectin from pomegranate peel residues and pectin prepared with method | |
| CN112094715A (en) | Method for preparing wine by utilizing cyperus cake meal through solid state fermentation | |
| CN102090500A (en) | Extraction method of medicinal and edible plant leaf protein and SOD (Super Oxide Dlsmutase) | |
| CN114717044A (en) | Processing method of peony flower liquid | |
| CN104435062B (en) | A kind of blueberry wine mud extract for inducing apoptosis on hepatic stellate cells and its preparation technology and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120222 Termination date: 20161229 |