CN107176987A - The method and device of Silk Reeling Waste Liquor recovery purifying sericin - Google Patents
The method and device of Silk Reeling Waste Liquor recovery purifying sericin Download PDFInfo
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- CN107176987A CN107176987A CN201710575908.9A CN201710575908A CN107176987A CN 107176987 A CN107176987 A CN 107176987A CN 201710575908 A CN201710575908 A CN 201710575908A CN 107176987 A CN107176987 A CN 107176987A
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- Prior art keywords
- sericin
- electric field
- silk reeling
- recovery purifying
- waste liquor
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/43504—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates
- C07K14/43563—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from insects
- C07K14/43586—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from insects from silkworms
Abstract
The invention belongs to technical field of waste water processing, and in particular to a kind of method of Silk Reeling Waste Liquor recovery purifying sericin.The method of Silk Reeling Waste Liquor recovery purifying sericin of the present invention is：Silk reeling wastewater removes impurity and inorganic ion through suction filtration and ultrafiltration；Utilize Ti/SnO2For anode material, platinum is that cathode material applies electric field, precipitates sericin in silk reeling wastewater using electric field action, obtains sericin；Obtained sericin is dissolved in aqueous medium after ultrasonic cleaning again, absolute ethyl alcohol is added, sericin after purification is obtained after centrifugation, supernatant.The method of the present invention is in the case of without chemical reagent, and the stability of colloid, isolated sericin can just be destroyed by applying low battery；This method extraction efficiency can reach 68% or so, and purity is 90.2%, and simple to operate, environment-friendly, with industrial applications meaning.
Description
Technical field
The invention belongs to technical field of waste water processing, and in particular to a kind of method of Silk Reeling Waste Liquor recovery purifying sericin
And device.
Background technology
Bombyx-mori Bave is a kind of natural protein fibre, it mainly by 70%~80% fibroin, 20%~30%
Silk gum and a small amount of wax and inorganic matter etc. are constituted.The sericin almost all in major part silk reeling wastewater is not reclaimed at present, is made
All excluded for waste liquid, because protein content is too high in sewage effluent, oxygen in water will largely be consumed by flowing into river course, be made
Water body loses self-purification capacity, causes substantial amounts of environmental pollution and energy waste.So, if processing and processing procedure in silk
It is middle efficiently to reclaim and exempt the pollution to environment using sericin, it will to produce huge economic benefit and society's effect
Benefit.Therefore, designing a kind of method that can extract sericin in silk reeling wastewater is extremely necessary.
Sericin such as serine, aspartic acid etc. containing amino acid of a large amount of side chains with hydrophilic radical, it is soluble in water in.Silkworm
Impurity in silk is mainly stored in silk gum.Sericin contains free carboxyl and amino, can interact and formed it is bipolar from
Son, with amphotericity, in the less solution of pH value, sericine exists with ion mode；In larger molten of pH value
In liquid, sericine exists in anion form, and the isoelectric point of sericin is 3.8~4.5, when solution value is close or critical
When isoelectric point, silk gum is in precipitation shape without in gel.
Sericine is a kind of valuable resource, the sericin being dissolved down during current reeling mill's fiber tow production
Matter is lost in the discharge of production waste water, and produces the major pollutants in waste water as filature, can cause bad to water environment
The recovery of sericine not only contributes to qualified discharge or the recycling of waste water in influence, silk reeling wastewater, will can also separate
Sericine out is used, and develops high added value byproduct.
The method of silk gum is extracted from waste water chemical leaching test and the major class of physics extraction method two.Wherein chemical leaching test has
Chemical coagulation process, acid-precipitation method and organic solvent precipitation method.Physics extraction method has centrifugal process, membrane separation process, freezing method and ion to hand over
Change method several.
The patent of Application No. 200710093091.8 discloses a kind of processing method of waste water containing sericin protein, and it is utilized
Silk gum itself occurs complexation reaction with metal and synthesizes sericin metal complex, is condensed by the use of this complex compound as flocculant
The silk gum in silk mill wastewater is precipitated, so as to carry out effective processing to waste water, is returned finally by the method low cost of weak acid scrubbing
Receive sericin.This method needs to add metallochemistry reagent, and cost is high, and subsequent treatment is complicated.
Application No. 201310073594.4, the China of entitled " intermediate processing of sericin in a kind of silk reeling wastewater "
Patent application is disclosed sequentially adds appropriate anhydrous citric acid and disodium hydrogen phosphate in silk reeling wastewater, and is stirred by agitator
Mix uniform, add appropriate tannic acid, then by heating and standing, so that sericin in silk reeling wastewater be precipitated out.
Although this method can obtain sericin, many chemical reagent are with the addition of, process is also more complicated.
The content of the invention
In view of this, it is an object of the invention to provide a kind of method from Silk Reeling Waste Liquor recovery purifying sericin, this
Method is simple to operate, and without chemical reagent, obtained sericin extraction efficiency and purity is high.
To achieve the above object, the technical scheme is that：
The method of Silk Reeling Waste Liquor recovery purifying sericin, comprises the following steps：
1) silk reeling wastewater removes impurity and inorganic ion through suction filtration and ultrafiltration, obtains treatment fluid；
2) Ti/SnO is utilized2For anode material, platinum is cathode material, in step 1) apply electric field in the treatment fluid, profit
Sericin is precipitated with electric field action, sericin is obtained；
3) by step 2) sericin be dissolved in after ultrasonic cleaning in aqueous medium, absolute ethyl alcohol is added, through centrifuging, going
Sericin after purification is obtained after supernatant.
The present invention has been respectively compared graphite, titanium plate electrode, Ti/SnO2As anode material feasibility, graphite material is in height
It can be dissolved in warm environment, titanium plate electrode price is higher oxidizable, Ti/SnO2Performance is stable, and operating voltage is small, service life
It is long, therefore selection Ti/SnO2It is used as anode material.With high-recovery, environmental and durable for main target, to the different factors of reaction
It is analyzed, finally gives the process conditions that a set of filature reclaims sericin.
Further, step 1) in ultrafiltration using interception be 3~4KDa ultrafiltration apparatus.
As a preferred embodiment, step 1) in ultrafiltration using interception be 3.5KDa ultrafiltration apparatus.
Further, step 2) electric field current density be 1.5~3.5mA/cm2, time of electric field action for 90~
120min。
As a preferred embodiment, step 2) current density of electric field is 2mA/cm2, the time of electric field action is 100min.
Further, step 3) in sericin and absolute ethyl alcohol volume ratio be 1:3~5.
As a preferred embodiment, step 3) in sericin and absolute ethyl alcohol volume ratio be 1:4.
Further, step 3) described in centrifugal condition be 2500~3500rpm, 3~8min.
As a preferred embodiment, step 3) described in centrifugal condition be 3000rpm, 5min.
Further, step 3) in purify the step of repeat 2~4 times.As a preferred embodiment, step 3) in purify the step of weight
It is multiple 3 times.
Further, methods described also includes step：4) by step 3) the obtained freeze-dried method of sericin, freezing is dry
Dry 2~4 days, obtain sericin product.
The second object of the present invention is that the device for providing a kind of utilization Silk Reeling Waste Liquor recovery purifying sericin reclaims pure
Change the method for sericin, described device is returned by the Suction filtration device being sequentially connected, enrichment facility, ultrafiltration apparatus, holding vessel, electric field
Receiving apparatus, isolate and purify device and drying device composition；The holding vessel discharging opening is provided with regulating valve, and the electric field reclaims dress
Install and be equipped with circulating line, the circulating line is provided with pump, the mother liquor of electric field retracting device enters storage by circulating line
Tank is deposited, the drying device is provided with temperature control equipment；Using the method for described device recovery purifying sericin, including with
Lower step：
1) silk reeling wastewater enters Suction filtration device through suction filtration removing impurity, and filtered feed liquid concentrates laggard in enrichment facility
Enter the ultrafiltration apparatus that interception is 3~4KDa and remove inorganic ion, obtain treatment fluid and be stored in holding vessel；
2) entered in electric field retracting device, made using electric field action by pipeline by controlling to adjust treatment fluid described in valve
Sericin is precipitated, and obtains sericin；
3) step 2) obtained sericin is dry by drying device after purification in 2~4 times by isolating and purifying device
Dry 2~4 days, obtain sericin product.
Further, the electric field retracting device utilizes Ti/SnO2For anode material, platinum is cathode material；The electric field is returned
Receiving apparatus is batch production.
Further, the device of the Silk Reeling Waste Liquor recovery purifying sericin passes through programme-control automated production.
The beneficial effects of the present invention are：
1) method for the Silk Reeling Waste Liquor recovery purifying sericin that the present invention is provided utilizes the colloidal nature of silk gum, in filature
Waste water applies with electric field, and sericin is precipitated using electric field action, and this method applies in the case of without chemical reagent
Low battery can just destroy the stability of colloid, isolated sericin；This method is simple, easy to operate, environment-friendly.
2) method mother liquid recycling of the invention, the sericin of recovery purifying is white powder, and effect is extracted after tested
Rate can reach 68% or so, and purity is 90.2%.
3) device for the Silk Reeling Waste Liquor recovery purifying sericin that the present invention is provided passes through programme-control automated production, place
The running efficiency for managing flow is higher, it is adaptable to large-scale industrial production, with industrial applications meaning.
Brief description of the drawings
Fig. 1 is the schematic diagram of the device of Silk Reeling Waste Liquor recovery purifying sericin of the present invention.
Embodiment
Hereinafter with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail.Unreceipted tool in preferred embodiment
The experimental method of concrete conditions in the establishment of a specific crime, generally according to normal condition, illustrated embodiment is to preferably be said to present disclosure
It is bright, but be not that present disclosure is only limitted to illustrated embodiment.So those skilled in the art are according to foregoing invention
Content carries out nonessential modifications and adaptations to embodiment, still falls within protection scope of the present invention.
Embodiment 1
The method of Silk Reeling Waste Liquor recovery purifying sericin, comprises the following steps：
1) silk reeling wastewater removes impurity through suction filtration, and filtered feed liquid removes impurity elimination through interception for 3.5KDa ultrafiltration apparatus
Matter and inorganic ion, obtain treatment fluid；
2) Ti/SnO is utilized2For anode material, platinum is cathode material, applies electric field, the electric current of field in the treatment fluid
Density is 2mA/cm2, the time of electric field action is 100min, precipitates sericin using electric field action, obtains sericin；
3) obtained sericin is dissolved in after ultrasonic cleaning in aqueous medium, adds the nothing of 4 times of sericin volume
Water-ethanol, through 3000rpm, 5min is centrifuged, is removed supernatant, is repeated 3 times, and collects precipitation；
4) freeze-drying is utilized, is freeze-dried 3 days, obtains sericin product.
Embodiment 2
The method of Silk Reeling Waste Liquor recovery purifying sericin, comprises the following steps：
1) silk reeling wastewater removes impurity through suction filtration, and filtered feed liquid removes impurity through interception for 4KDa ultrafiltration apparatus
And inorganic ion, obtain treatment fluid；
2) Ti/SnO is utilized2For anode material, platinum is cathode material, applies electric field, the electric current of field in the treatment fluid
Density is 2mA/cm2, the time of electric field action is 100min, precipitates sericin using electric field action, obtains sericin；
3) obtained sericin is dissolved in after ultrasonic cleaning in aqueous medium, adds 4.5 times of sericin volume
Absolute ethyl alcohol, through 3000rpm, 5min is centrifuged, is removed supernatant, is repeated 3 times, and collects precipitation；
4) freeze-drying is utilized, is freeze-dried 3 days, obtains sericin product.
Embodiment 3
The method of Silk Reeling Waste Liquor recovery purifying sericin, comprises the following steps：
1) silk reeling wastewater removes impurity through suction filtration, and filtered feed liquid removes impurity elimination through interception for 3.5KDa ultrafiltration apparatus
Matter and inorganic ion, obtain treatment fluid；
2) Ti/SnO is utilized2For anode material, platinum is cathode material, applies electric field, the electric current of field in the treatment fluid
Density is 2mA/cm2, the time of electric field action is 100min, precipitates sericin using electric field action, obtains sericin；
3) obtained sericin is dissolved in after ultrasonic cleaning in aqueous medium, adds 3.5 times of sericin volume
Absolute ethyl alcohol, through 3200rpm, 5min is centrifuged, is removed supernatant, is repeated 3 times, and collects precipitation；
4) freeze-drying is utilized, is freeze-dried 3 days, obtains sericin product.
Comparative example 4
The anode material for applying electric field is graphite or titanium plate electrode, other conditions be the same as Example 1.
It has been respectively compared graphite, titanium plate electrode, Ti/SnO2As for anode material feasibility, a period of time is used to find
Graphite material can dissolve in hot environment, and titanium plate electrode price is higher oxidizable, Ti/SnO2Performance is stable, work electricity
Pressure is small, and service life is long, therefore selection Ti/SnO2It is used as anode material.
Embodiment 5
It is shown in Figure 1, the device of Silk Reeling Waste Liquor recovery purifying sericin：Described device is filled by the suction filtration being sequentially connected
Put 1, enrichment facility 2, ultrafiltration apparatus 3, holding vessel 4, electric field retracting device 5, isolate and purify device 6 and drying device 7 is constituted；Institute
State the discharging opening of holding vessel 4 and be provided with regulating valve 8, the electric field retracting device is provided with circulating line 9, and the circulating line 9 is set
Pump 10 is equipped with, the mother liquor of electric field retracting device 5 enters holding vessel 4 by circulating line 9, and the drying device 7 is provided with temperature
Spend control device；
The electric field retracting device 5 utilizes Ti/SnO2For anode material, platinum is cathode material；The electric field retracting device
For batch production, the device of the Silk Reeling Waste Liquor recovery purifying sericin passes through programme-control automated production.
Embodiment 6
Utilize the method for the device recovery purifying sericin of Silk Reeling Waste Liquor recovery purifying sericin, including following step
Suddenly：
1) silk reeling wastewater enters Suction filtration device 1 through suction filtration removing impurity, after filtered feed liquid is concentrated in enrichment facility 2
Inorganic ion is removed for 3~4KDa ultrafiltration apparatus 3 into interception, treatment fluid is obtained and is stored in holding vessel 4；
2) entered by controlling to adjust treatment fluid described in valve 8 by pipeline in electric field retracting device 5, utilize electric field action
Sericin is precipitated, sericin is obtained；
3) step 2) obtained sericin is by isolating and purifying after purification by drying device 7 for 2~4 times of device 6
Dry 2~4 days, obtain sericin product.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to compared with
The present invention is described in detail good embodiment, it will be understood by those within the art that, can be to skill of the invention
Art scheme is modified or equivalent substitution, and without departing from the objective and scope of technical solution of the present invention, it all should cover at this
Among the right of invention.
Claims (10)
1. the method for Silk Reeling Waste Liquor recovery purifying sericin, it is characterised in that comprise the following steps：
1) silk reeling wastewater removes impurity and inorganic ion through suction filtration and ultrafiltration, obtains treatment fluid；
2) Ti/SnO is utilized2For anode material, platinum is cathode material, in step 1) apply electric field in the treatment fluid, utilize electric field
Effect precipitates sericin, obtains sericin；
3) by step 2) sericin be dissolved in after ultrasonic cleaning in aqueous medium, absolute ethyl alcohol is added, through centrifuging, removing supernatant
Sericin after purification is obtained after liquid.
2. ultrafiltration is the super of 3~4KDa using interception according to the method described in claim 1, it is characterised in that step 1)
Filter device.
3. the current density of electric field is 1.5~3.5mA/cm according to the method described in claim 1, it is characterised in that step 2)2,
The time of electric field action is 90~120min.
4. the volume ratio of sericin and absolute ethyl alcohol is according to the method described in claim 1, it is characterised in that step 3)
1:3~5.
5. the centrifugal condition described according to the method described in claim 1, it is characterised in that step 3) is 2500~3500rpm,
3~8min.
6. the step of being purified according to the method described in claim 1, it is characterised in that step 3) repeats 2~4 times.
7. according to the method described in claim 1, it is characterised in that methods described also includes step：
4) by step 3) the obtained freeze-dried method of sericin, it is freeze-dried 2~4 days, obtains sericin product.
8. the method for the device recovery purifying sericin using Silk Reeling Waste Liquor recovery purifying sericin, it is characterised in that institute
Device is stated by the Suction filtration device (1) being sequentially connected, enrichment facility (2), ultrafiltration apparatus (3), holding vessel (4), electric field retracting device
(5) device (6) and drying device (7) composition, are isolated and purified；Holding vessel (4) discharging opening is provided with regulating valve (8), described
Electric field retracting device is provided with circulating line (9), and the circulating line (9) is provided with pump (10), the mother of electric field retracting device (5)
Liquid enters holding vessel (4) by circulating line (9), and the drying device (7) is provided with temperature control equipment；Utilize the dress
The method for putting recovery purifying sericin, comprises the following steps：
1) silk reeling wastewater enters Suction filtration device (1) through suction filtration removing impurity, after filtered feed liquid is concentrated in enrichment facility (2)
Inorganic ion is removed for 3~4KDa ultrafiltration apparatus (3) into interception, treatment fluid is obtained and is stored in holding vessel (4)；
2) entered by controlling to adjust valve (8) treatment fluid by pipeline in electric field retracting device (5), utilize electric field action
Sericin is precipitated, sericin is obtained；
3) step 2) obtained sericin is by isolating and purifying after purification by drying device (7) for 2~4 times of device (6)
Dry 2~4 days, obtain sericin product.
9. method according to claim 8, it is characterised in that the electric field retracting device (5) utilizes Ti/SnO2For anode
Material, platinum is cathode material；The electric field retracting device (5) is batch production.
10. method according to claim 8, it is characterised in that the device of the Silk Reeling Waste Liquor recovery purifying sericin
Pass through programme-control automated production.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710575908.9A CN107176987A (en) | 2017-07-14 | 2017-07-14 | The method and device of Silk Reeling Waste Liquor recovery purifying sericin |
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| CN201710575908.9A CN107176987A (en) | 2017-07-14 | 2017-07-14 | The method and device of Silk Reeling Waste Liquor recovery purifying sericin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108164059A (en) * | 2018-01-30 | 2018-06-15 | 浙江工业大学膜分离与水处理协同创新中心湖州研究院 | A kind of embrane method processing cocoon boiling wastewater and the method for recycling sericin |
| CN108409847A (en) * | 2018-03-05 | 2018-08-17 | 苏州先蚕丝绸有限公司 | A kind of recovery method of silk silk gum |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108164059A (en) * | 2018-01-30 | 2018-06-15 | 浙江工业大学膜分离与水处理协同创新中心湖州研究院 | A kind of embrane method processing cocoon boiling wastewater and the method for recycling sericin |
| CN108409847A (en) * | 2018-03-05 | 2018-08-17 | 苏州先蚕丝绸有限公司 | A kind of recovery method of silk silk gum |
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Inventor after: Zhou Chan Inventor after: Pu Shihua Inventor after: Lv Jinfeng Inventor after: Li Jin Inventor after: Wang Jieping Inventor before: Zhou Chan |
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Application publication date: 20170919 |