CN102746420A - Method for recovering pectin from orange can processing wastewater - Google Patents
Method for recovering pectin from orange can processing wastewater Download PDFInfo
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- CN102746420A CN102746420A CN2012102612376A CN201210261237A CN102746420A CN 102746420 A CN102746420 A CN 102746420A CN 2012102612376 A CN2012102612376 A CN 2012102612376A CN 201210261237 A CN201210261237 A CN 201210261237A CN 102746420 A CN102746420 A CN 102746420A
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Abstract
The invention belongs to the field of changing food processing wastewater into resources, and discloses a method for separating and extracting pectin from orange can wastewater. The method comprises the following steps: a. pretreatment: adding a decolorant to acid and alkali treatment wastewater in orange can production wastewater, decolorizing under the condition of 60-90 DEG C for 10-60min, and carrying out solid-liquid separation to obtain clear liquid; b. adjusting the pH value of the clear liquid obtained in the step a to 2-5, adding ferric sulfate, heating in a water bath under the condition of 50-80 DEG C for 30-90min, and centrifuging to obtain pectate precipitate; and c. adding desalination liquid to the pectate precipitate, stirring and desalinating for 30-90min, centrifugally separating, washing the precipitate with alcohol for 2-3 times, washing with clean water for 2-3 times, and finally vacuum-drying to obtain the pectin product. According to the invention, recovery and reutilization of pectin are achieved, the pectin concentration in the wastewater is reduced, the treatment difficulty of the orange can wastewater is reduced and the economic benefit is high.
Description
Technical field
The invention belongs to food processing wastewater changing waste into resources field, be specifically related to a kind of method of utilizing oranges and tangerines can waste water separation and Extraction to reclaim pectin.
Background technology
Oranges and tangerines can factory effluent mainly contains: (1) oranges and tangerines pretreated waste water (scalding the soaked in water in hot water, peeling and the distinguish process of tangerine) contains the tangerine oil, pectin of stripping on a spot of silt and the orange peel etc.(2) acid-alkali treatment water, pectin content is very high, can reach about 4000 mg/L.(3) the later check waste water of tangerine lobe classification waste water and classification.(4) following process waste water (waste water that tinning envelope jar and sterilization produce).Contain a large amount of pectin in the oranges and tangerines can factory effluent, pectin is a kind of polysaccharide polymer of complicacy, is a kind of water-soluble plant glue, has gelling and emulsifying effect preferably.Have a wide range of applications in fields such as food, medicine, makeup, weaving and printing and dyeing.According to incompletely statistics, more than the annual about 1500t of pectin demand of China.Wherein, most of from external import.
The pectin tack is very strong, can adhere to and wrap up zoogloea, is difficult to biolysis; Pectin has nature toughness, is prone to make mud pulp or pasty state, causes the dehydration difficulty.Existing materialization and biochemical combined treatment process are relatively poor to the removal effect of pectin in the oranges and tangerines can factory effluent, make oranges and tangerines can production wastewater treatment become the major obstacles of puzzlement enterprise development gradually.
To above situation, the novel technical method that extracts pectin a kind of acid-alkali treatment waste water of process of producing from the oranges and tangerines can need be provided at present, both reached the pectin recycling, can reduce the concentration of pectin in the waste water again, reduce the intractability of oranges and tangerines can waste water.
Summary of the invention
The purpose of this invention is to provide a kind of method that reclaims pectin of from oranges and tangerines can waste water, extracting, both reached the pectin recycling, can reduce the concentration of pectin in the waste water again, reduce the intractability of oranges and tangerines can waste water.
In order to solve the problems of the technologies described above, the present invention is able to solve through following technical proposals:
Utilize oranges and tangerines can waste water to extract the method that reclaims pectin, method is following:
A, pre-treatment: add discoloring agent in the acid-alkali treatment waste water in oranges and tangerines can factory effluent, decolouring 10-60 min under 60-90 ℃ the condition, solid-liquid separation obtains clear liquid;
B: the clear liquid pH value that obtains among the regulating step a is 2-5, adds ferric sulfate, heating in water bath 30-90min under the 50-80 ℃ of condition, the centrifugal pectate deposition that obtains;
C: in the pectate deposition, add demineralised liquid, stir desalination 30-90min, spinning, throw out is through alcohol washing 2-3 time, again through clear water washing 2-3 time, after vacuum-drying obtains pectin product.
As preferably, the rotating speed among the described step b in the centrifugal process is 3000-8000 r/min, and centrifugation time is 10-30 min.
As preferably, the percent weight in volume of the ferric sulfate that adds in the described step b clear liquid is 2%-8%.
As preferably, the composition volume ratio of demineralised liquid is following among the described step c: hydrochloric acid: ethanol: water=3:60:37.
As preferably, the consumption of demineralised liquid is 1 with oranges and tangerines can factory effluent volume of water sample ratio among the described step c: (1-1.2).
As preferably, pure washing process adopts 70% ethanol to wash among the described step c, in order to remove alcohol dissolubility impurity.
As preferably, described discoloring agent is a gac, and the bulking value ratio that its add-on accounts for total waste water is 1.0%-2.0%.
As preferably, among the described step c in the process of vacuum drying temperature be 40-60 ℃, be 4-6h time of drying.
As preferably, described whipping appts adopts magnetic stirring apparatus.
The present invention has significant technique effect owing to adopted above technical scheme:
The present invention is directed to the more hard to manage and rare realistic problem of pectin product of existing oranges and tangerines can factory effluent, propose a kind of feasible solution, adopt the molysite salting-out process to extract and reclaim the pectin in the oranges and tangerines can factory effluent.
The traditional method of producing pectin is aluminium salt salting-out process and ethanol precipitation, produces pectin with aluminium salt salting-out process and compares, and the detrimentally affect that the method for utilizing molysite to extract pectin disclosed by the invention can avoid aluminium that human body is produced, and also the pectin productive rate is also higher;
Compare with ethanol precipitation, the method for utilizing molysite to extract pectin disclosed by the invention can significantly reduce consumption of ethanol, and production cost is low, and the recovery is high, and the recovery can reach about 70%, has wide development and application prospect.
Description of drawings
Fig. 1 is the process flow sheet that molysite salting-out process of the present invention extracts pectin.
Embodiment
The present invention is described in further detail with embodiment below in conjunction with accompanying drawing 1:
Embodiment 1
Oranges and tangerines can factory effluent is the factory effluent that Hunan Province oranges and tangerines canning factory provides, and wherein the pH value of s.t. spent process water is 1 ~ 3, and the pH value of alkaline purification spent process water is 6 ~ 9, and waste water quality is seen table 1.
The staple of table 1 acid-alkali treatment waste water
| Wastewater source | SS（mg/L） | COD（mg/L） | BOD（mg/L） | Pectin content (mg/L) |
| S.t. waste water | 950 | 5500 | 2300 | 2700 |
| Alkaline purification waste water | 760 | 4350 | 2000 | 4100 |
Below in conjunction with Figure of description the present invention is done into-goes on foot explanation:
According to operating procedure of the present invention, the molysite salting-out process shown in accompanying drawing 1 extracts the technical process of pectin, carries out the pectin factory effluent is extracted pectin.Its key step is following:
1) the decolouring pre-treatment of oranges and tangerines can factory effluent
Because water sample is faint yellow, can influence the quality of the pectin that extracts, so before extraction pectin, must be to the waste water pre-treatment of decolouring.In the ratio of 1.2% (w/v), add gac in the acid-alkali treatment waste water in oranges and tangerines can factory effluent, decolouring 20 min under 80 ℃ condition, solid-liquid separation obtains clear liquid.
2) the molysite salting-out process extracts pectin
The pH that regulates above-mentioned gained clear liquid is 5, in the ratio of 6% (w/v), adds ferric sulfate, heating 1 h under 70 ℃ condition, and spinning (rotating speed 5000 r/min, times 10 min) obtains the pectate deposition.(regulating the used material of pH is ammoniacal liquor and hydrochloric acid).
3) desalination
In above-mentioned pectate deposition; Add the demineralised liquid that equates with the waste water volume of water sample, the composition of demineralised liquid is a hydrochloric acid: ethanol: water=3:60:37 (volume ratio), stir desalination 1 h; After the spinning; Priority adds 70% ethanol and deionized water in solid, washs 2 ~ 3 times, obtains pectin solution.
4) extract the pectin finished product
Behind above-mentioned pectin solution recentrifuge after desalination alcohol is washed, what obtain is deposited in vacuum-drying 5h under 45 ℃ of conditions, obtains pectin product.Weighing obtains pectin product; The result shows that the extraction yield of pectin can reach about 70%.
The present invention compares each experiment condition contrast with traditional aluminium salt salting-out process and sees table 2 with ethanol precipitation.
Table 2 Different Extraction Method is extracted the pectin contrast
| Process for extracting | Deposition pH | ST (min) | Precipitation temperature (℃) | Amount of ethanol (with the volume of water sample ratio) | The pectin product yield |
| Aluminium salt salting-out process | 5.0 | 60 | 60 | 1:1 | 63.2% |
| Ethanol precipitation | 3.5~4.0 | 30 | 40 | 2:1 | 69.5% |
| The molysite salting-out process | 5.0 | 60 | 70 | 1:1 | 62.3% |
Can find out that by table 2 result the pectin extraction yield of ethanol precipitation is the highest, but amount of ethanol is also very big, and ethanol precipitation need concentrate to water sample, thereby consume more energy, increase production cost; Aluminium salt salting-out process extraction yield is higher than molysite salting-out process, but in demineralising process, dealuminzation thoroughly can not cause aluminium salt residual, and aluminium has certain hazardness to human body.And the sulphate of iron precipitator method are compared with two kinds of traditional methods; The detrimentally affect that not only can avoid aluminium that human body is produced, and can significantly reduce consumption of ethanol, reduce production costs; The recovery is also very high, is the technological method that pectin is reclaimed in the very wide extraction of a kind of development and application prospect.
In a word, the above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to the covering scope of patent of the present invention.
Claims (9)
1. utilize oranges and tangerines can waste water to extract the method for pectin, it is characterized in that said method is following:
A, pre-treatment: add discoloring agent in the acid-alkali treatment waste water in oranges and tangerines can factory effluent, decolouring 10-60 min under 60-90 ℃ the condition, solid-liquid separation obtains clear liquid;
B: the clear liquid pH value that obtains among the regulating step a is 2-5, adds ferric sulfate, heating in water bath 30-90min under the 50-80 ℃ of condition, the centrifugal pectate deposition that obtains;
C: in the pectate deposition, add demineralised liquid, stir desalination 30-90min, spinning, throw out is through alcohol washing 2-3 time, again through clear water washing 2-3 time, after vacuum-drying obtains pectin product.
2. the method for utilizing oranges and tangerines can waste water to extract pectin according to claim 1, it is characterized in that: the rotating speed among the described step b in the centrifugal process is 3000-8000 r/min, centrifugation time is 10-30 min.
3. the method for utilizing oranges and tangerines can waste water to extract pectin according to claim 1, it is characterized in that: the percent weight in volume of the ferric sulfate that adds in the described step b clear liquid is 2%-8%.
4. the method for utilizing oranges and tangerines can waste water to extract pectin according to claim 1, it is characterized in that: the composition volume ratio of demineralised liquid is following among the described step c: hydrochloric acid: ethanol: water=3:60:37.
5. the method for utilizing oranges and tangerines can waste water to extract pectin according to claim 1, it is characterized in that: the consumption of demineralised liquid is 1 with oranges and tangerines can factory effluent volume of water sample ratio among the described step c: (1-1.2).
6. the method for utilizing oranges and tangerines can waste water to extract pectin according to claim 1, it is characterized in that: pure washing process adopts 70% ethanol to wash among the described step c, in order to remove alcohol dissolubility impurity.
7. the method for utilizing oranges and tangerines can waste water to extract pectin according to claim 1, it is characterized in that: described discoloring agent is a gac, the bulking value ratio that its add-on accounts for total waste water is 1.0%-2.0%.
8. the method for utilizing oranges and tangerines can waste water to extract pectin according to claim 1 is characterized in that: among the described step c in the process of vacuum drying temperature be 40-60 ℃, be 4-6h time of drying.
9. the method for utilizing oranges and tangerines can waste water to extract pectin according to claim 1 is characterized in that: described whipping appts adopts magnetic stirring apparatus.
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| CN2012102612376A CN102746420A (en) | 2012-07-26 | 2012-07-26 | Method for recovering pectin from orange can processing wastewater |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103122039A (en) * | 2013-03-05 | 2013-05-29 | 浙江大学 | Process for extracting pectin from acid discharge liquor generated in canned citrus production |
| CN103122038A (en) * | 2013-03-05 | 2013-05-29 | 浙江大学 | Process for extracting pectin from alkali discharge liquor generated in canned citrus production |
| CN105820269A (en) * | 2016-05-27 | 2016-08-03 | 浙江大学 | Method for recycling pectin in orange can acid treatment water |
| CN105859909A (en) * | 2016-05-27 | 2016-08-17 | 浙江大学 | Method for recovering pectin from canned citrus alkali treatment water |
| CN107640807A (en) * | 2017-09-19 | 2018-01-30 | 浙江树人学院（浙江树人大学） | A kind of pretreatment of citrus can production waste water and the method for reclaiming pectin simultaneously |
| CN111499772A (en) * | 2019-06-30 | 2020-08-07 | 浙江大学 | Method for co-recovering alkaline water/acid water and pectin in orange peel in orange can processing |
| CN114380926A (en) * | 2021-12-21 | 2022-04-22 | 浙江工商大学 | Method for recovering citrus pectin from citrus processing water and use thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1884143A (en) * | 2006-07-11 | 2006-12-27 | 浙江省环境保护科学设计研究院 | Process for treating industrial wastewater in production of canned mandarin orange |
-
2012
- 2012-07-26 CN CN2012102612376A patent/CN102746420A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1884143A (en) * | 2006-07-11 | 2006-12-27 | 浙江省环境保护科学设计研究院 | Process for treating industrial wastewater in production of canned mandarin orange |
Non-Patent Citations (1)
| Title |
|---|
| 汪海波等: "柑橘皮果胶的改进提取工艺研究", 《食品科学》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103122039A (en) * | 2013-03-05 | 2013-05-29 | 浙江大学 | Process for extracting pectin from acid discharge liquor generated in canned citrus production |
| CN103122038A (en) * | 2013-03-05 | 2013-05-29 | 浙江大学 | Process for extracting pectin from alkali discharge liquor generated in canned citrus production |
| CN105820269A (en) * | 2016-05-27 | 2016-08-03 | 浙江大学 | Method for recycling pectin in orange can acid treatment water |
| CN105859909A (en) * | 2016-05-27 | 2016-08-17 | 浙江大学 | Method for recovering pectin from canned citrus alkali treatment water |
| CN105859909B (en) * | 2016-05-27 | 2019-01-25 | 浙江大学 | A method of pectin in recycling citrus can alkali process water |
| CN105820269B (en) * | 2016-05-27 | 2019-01-25 | 浙江大学 | A method of pectin in recycling citrus can acid processing water |
| CN107640807A (en) * | 2017-09-19 | 2018-01-30 | 浙江树人学院（浙江树人大学） | A kind of pretreatment of citrus can production waste water and the method for reclaiming pectin simultaneously |
| CN111499772A (en) * | 2019-06-30 | 2020-08-07 | 浙江大学 | Method for co-recovering alkaline water/acid water and pectin in orange peel in orange can processing |
| CN111499772B (en) * | 2019-06-30 | 2021-05-11 | 浙江大学 | Method for co-recovering alkaline water/acid water and pectin in orange peel in orange can processing |
| CN114380926A (en) * | 2021-12-21 | 2022-04-22 | 浙江工商大学 | Method for recovering citrus pectin from citrus processing water and use thereof |
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