CN108164059A - A kind of embrane method processing cocoon boiling wastewater and the method for recycling sericin - Google Patents
A kind of embrane method processing cocoon boiling wastewater and the method for recycling sericin Download PDFInfo
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Abstract
The invention discloses biologic treating techniques, specifically criticize a kind of embrane method processing cocoon boiling wastewater and the method for recycling sericin.The present invention is mixed activated carbon, sodium carboxymethylcellulose, Kynoar by preparing the preparations of specific activated carbon electrodes, adds in N methyl pyrrolidones, and coated in nickel foam；It is prepared；The processes such as adsorption treatment, parsing are carried out to cocoon boiling wastewater to electric adsorption device again.Protein functional is destroyed it is an advantage of the invention that can reduce, the recycling of sericin in waste water is realized, prepares ease of solubility sericin powder, may be used in additional byproduct, realizes the recycling of silk waste water.This method technological process is simple, the rate of recovery is high, cost is relatively low, energy conservation and environmental protection, is suitble to large-scale industrial production.
Description
Technical field：
The invention belongs to biotechnologies, and in particular to a kind of embrane method processing cocoon boiling wastewater and the side for recycling sericin
Method.
Background technology：
Silk mill in Primary Processing since throwing and the needs of textile technology, silk gum are not utilized, but gradually
It is taken off.River such as is directly discharged into without processing, the dissolved oxygen in water will be consumed in large quantities, the COD for leading to water is tight
Weight is exceeded, destroys the water quality of original water, local natural water is caused centainly to pollute.
Traditional Methods of Sericin Recycling has acid-precipitation method, chemical coagulation process, freezing and membrane separation process.Wherein acid-precipitation method is silk gum
Most common method in recycling, the amphotericity of its foundation sericin reach extraction silk gum by adjusting solution ph
Purpose.The advantages of this method is that technological process is fairly simple, and the silk gum of recycling is relatively pure, but the rate of recovery is not high, and resistance to equipment
Acid requirement is higher.The colloidal nature of its foundation sericin of chemical coagulation process, flocculant is added in sericine waste water
Such as it polymerize AlCl3, alum and CaC12Saturated solution etc. is to destroy the stabilization of protein adhesive liquid solution, so as to which sericin be made to sink
It forms sediment, separation.But silk gum purity and the rate of recovery are very low.Freezing method can condense into frozen glue shape according to protein solution when temperature declines
State generates the characteristics of gel.In the case where pH value is 7, temperature is -24 DEG C, frost 11h opens the protein particulate disperseed originally in waste water
Beginning is joined to one another, and forms complicated reticular structure, silk gum particle is detached from colloidal solution in the form of flocculent deposit
Out.But the sericin purity of recycling is not high.Membrane separation process is big according to protein molecular weight, is sieved according to film surface aperture
Mechanism, the retardance mechanism of fenestra resistance and film surface and fenestra select suitable filter membrane, to silk gum to an adsorption mechanism of particle
Albumen carries out selective filter extraction, and membrane separation technique will realize industrialized production there are the problems such as of high cost, fenestra easily blocks
Also to solve many technical barriers.
The present invention can carry out sericin in waste water high-recovery profit using technical methods such as Electro Sorb, membrane distillations
With, and raffinate is subjected to processing and reaches national grade one discharge standard.Wherein activated carbon Electro Sorb technology is raw water in yin, yang two
Pole flowing is acted on by electric field, and the charged particle in stoste is active respectively to the electrode transfer in oppositely charged direction
Carbon resistance rod is adsorbed and is stored in electric double layer, and with increasing for electrode adsorption charged ion, charged ion is in activated carbon electrodes table
Face enrichment concentration finally makes sericin absorption on activated carbon electrodes.Membrane distillation is that membrane technology is combined with distillation process
Membrane separating process, it is using dewatering microporous film as medium, and under the action of the steam pressure difference of film both sides, volatile component is to steam in feed liquid
Vapour form penetrates fenestra, so as to fulfill the purpose of separation.In the art, membrane distillation by parse protein liquid into moisture evaporation,
Achieve the purpose that concentration.
This technique, which can be reduced, destroys protein functional, realizes the recycling of sericin in waste water, prepares
Ease of solubility sericin powder may be used in additional byproduct, realize the recycling of silk waste water.This method technological process letter
Single, rate of recovery height, cost are relatively low, and energy conservation and environmental protection is suitble to large-scale industrial production.
Invention content
The present invention handles cocoon boiling wastewater and the method for recycling sericin for a kind of embrane method, utilizes the electrical property of sericin
Matter, the sericin in waste water is adsorbed using Electro Sorb method, the sericin of high-purity is obtained using parsing, in technical process
Waste water reaches discharge standard through processing, has many advantages, such as that low energy consumption, the rate of recovery is high, easy to operate, energy conservation and environmental protection, is suitble to industrialization
Production.
The present invention is achieved by the following technical programs：
A kind of embrane method processing cocoon boiling wastewater and the method for recycling sericin, include the following steps：
(1) preparation of activated carbon electrodes
Property carbon powder is cleaned with deionized water to water conductivity and is adjusted to 10~30 μ s/cm, is subsequently placed in 100 DEG C of baking ovens
Interior drying, then activated carbon, sodium carboxymethylcellulose, Kynoar, than mixing, are then added in quantitative according to certain mass
N-Methyl pyrrolidone makes it uniformly mix with 24~48h of magnetic stirrer.Said mixture is coated using coating device
In nickel foam.The electrode of preparation is placed in baking oven and is dried.It is for use that activated carbon coating electrode finished product is made in last tabletting.
(2) cocoon boiling wastewater is first filtered into removal partial impurities with microporous membrane filters, is then centrifuged for isolated supernatant,
Supernatant pH value range is adjusted 10~14 with NaOH solution, because sericin is amphiprotic substance, in the solution that pH value is larger
In sericin it is negatively charged, then by step (1) prepare activated carbon electrodes be used for electric adsorption device cathode, expanded sheet metal
Anode as electric adsorption device, is adsorbed, adsorption time 48h, and experimental result finds that the Electro Sorb time is longer, recycling
Sericin content it is higher.Making parsing solution with 65~85 DEG C of water or sodium hydroxide solution will be inhaled on activated carbon electrodes plate
Attached sericin is parsed, and 1.0~2.0h of parsing obtains parsing protein solution, and the protein solution for finally obtaining parsing is again
Sericin powder is obtained by membrane distillation concentration, Freeze Drying Technique.And the surplus solution after Electro Sorb is subjected to coagulating sedimentation,
The water quality discharge of cocoon boiling wastewater after processing is made to meet wastewater discharge standard requirement.
Wherein protein content is measured using K9840 types Protein Analyzer, according to GB 5009.5-2010 methods
Add in 0.2g CuSO4、6g K2SO4、20ml H2SO4It is put into resolution test tube with 10g stostes and clears up 2.5h, in test tube to be cleared up
Solution is clarified, and is put into K9840 type Protein Analyzers and is measured.
Preferably, a kind of embrane method processing cocoon boiling wastewater and the method for recycling sericin, described in Electro Sorb process
Middle electric current is 0.05A, voltage 60V.
Advantageous effect：It can reduce and protein functional is destroyed, realize the recycling of sericin in waste water, prepare
Go out ease of solubility sericin powder, may be used in additional byproduct, realize the recycling of silk waste water.This method technological process letter
Single, rate of recovery height, cost are relatively low, and energy conservation and environmental protection is suitble to large-scale industrial production.
Specific embodiment
With reference to example, the present invention will be further described, but protection scope of the present invention is not limited to this：
Comparative example 1
(1) cocoon boiling wastewater 1.5L micro-pore-film filtrations are taken, the solution after filtering is centrifuged to obtain supernatant and precipitation, are used
The NaOH solution of 1mol/L adjusts supernatant pH to 11, measures the sericin content in solution with Kjeldahl's method, obtains 1L
Protein content in supernatant is 5.25g, and sericin content is 0.21g in precipitation, so not considering sericin in precipitation
Content.
(2) using ordinary electrode as the cathode of electric adsorption device, anode of the steel plate as electric adsorption device takes step (1)
Middle supernatant 1L carries out Electro Sorb adsorption time 48h, and the sericin adsorbed on ordinary electrode is parsed, and parses solution temperature
It is 85 DEG C to spend, and the parsing time is 2.0h, then obtained parsing solution Kjeldahl's method is measured to the silk gum in parsing solution
Protein content obtains the sericin content in parsing solution as 2.80g, the rate of recovery 53%.
Embodiment 1
(1) property carbon powder is cleaned with deionized water to water conductivity and is down to 10us/cm, be subsequently placed in 100 DEG C of baking ovens
Drying, then by activated carbon, sodium carboxymethylcellulose, Kynoar according to 8:1:1 mass ratio mixing, then adds in quantitative
N-Methyl pyrrolidone makes it uniformly mix with magnetic stirrer 48h.Said mixture is coated in bubble using coating device
On foam nickel.The electrode of preparation is placed in baking oven and is dried.It is for use that activated carbon coating electrode finished product is made in last tabletting.
(2) cocoon boiling wastewater 1.5L micro-pore-film filtrations are taken, the solution after filtering is centrifuged to obtain supernatant and precipitation, are used
The NaOH solution of 1mol/L adjusts supernatant pH to 11, measures the sericin content in solution with Kjeldahl's method, obtains 1L
Protein content in supernatant is 5.25g, and sericin content is 0.21g in precipitation, so not considering sericin in precipitation
Content.
(3) using the activated carbon electrodes in step (1) as the cathode of electric adsorption device, expanded sheet metal is as electric adsorption device
Anode, supernatant 1L is taken in step (2) to carry out Electro Sorb adsorption time 48h, the sericin that will be adsorbed on activated carbon electrodes
It is parsed, parsing solution temperature is 85 DEG C, and the parsing time is 2.0h, then surveys obtained parsing solution with Kjeldahl's method
Sericin content in amount parsing solution obtains the sericin content in parsing solution as 4.80g, the rate of recovery 91%.
Embodiment does not form the limit to the scope of the present invention only to facilitate understand technical scheme of the present invention
System, any letter that every technical spirit without departing from technical solution of the present invention perhaps according to the present invention makees above scheme
Single modification, equivalent variations and modification, still fall within the scope of the present invention.
Embodiment 2
(1) property carbon powder is cleaned with deionized water to water conductivity and is down to 20us/cm, be subsequently placed in 100 DEG C of baking ovens
Drying, then by activated carbon, sodium carboxymethylcellulose, Kynoar according to 9:1:1 mass ratio mixing, then adds in quantitative
N-Methyl pyrrolidone makes it uniformly mix with magnetic stirrer 48h.Said mixture is coated in bubble using coating device
On foam nickel.The electrode of preparation is placed in baking oven and is dried.It is for use that activated carbon coating electrode finished product is made in last tabletting.
(2) cocoon boiling wastewater 1.5L micro-pore-film filtrations are taken, the solution after filtering is centrifuged to obtain supernatant and precipitation, are used
The NaOH solution of 1mol/L adjusts supernatant pH to 11, measures the sericin content in solution with Kjeldahl's method, obtains 1L
Protein content in supernatant is 5.25g, and sericin content is 0.21g in precipitation, so not considering sericin in precipitation
Content.
(3) using the activated carbon electrodes in step (1) as the cathode of electric adsorption device, expanded sheet metal is as electric adsorption device
Anode, supernatant 1L is taken in step (2) to carry out Electro Sorb adsorption time 48h, the sericin that will be adsorbed on activated carbon electrodes
It is parsed, parsing solution temperature is 75 DEG C, and the parsing time is 1.0h, then surveys obtained parsing solution with Kjeldahl's method
Sericin content in amount parsing solution obtains the sericin content in parsing solution as 4.6g, the rate of recovery 87.6%.
Embodiment does not form the limit to the scope of the present invention only to facilitate understand technical scheme of the present invention
System, any letter that every technical spirit without departing from technical solution of the present invention perhaps according to the present invention makees above scheme
Single modification, equivalent variations and modification, still fall within the scope of the present invention.
Embodiment 3
(1) property carbon powder is cleaned with deionized water to water conductivity and is down to 30us/cm, be subsequently placed in 100 DEG C of baking ovens
Drying, then by activated carbon, sodium carboxymethylcellulose, Kynoar according to 10:1:1 mass ratio mixing, then adds in quantitative
N-Methyl pyrrolidone, it is made uniformly to mix with magnetic stirrer 48h.Said mixture is coated in using coating device
In nickel foam.The electrode of preparation is placed in baking oven and is dried.It is for use that activated carbon coating electrode finished product is made in last tabletting.
(2) cocoon boiling wastewater 1.5L micro-pore-film filtrations are taken, the solution after filtering is centrifuged to obtain supernatant and precipitation, are used
The NaOH solution of 1mol/L adjusts supernatant pH to 11, measures the sericin content in solution with Kjeldahl's method, obtains 1L
Protein content in supernatant is 5.25g, and sericin content is 0.21g in precipitation, so not considering sericin in precipitation
Content.
(3) using the activated carbon electrodes in step (1) as the cathode of electric adsorption device, expanded sheet metal is as electric adsorption device
Anode, supernatant 1L is taken in step (2) to carry out Electro Sorb adsorption time for 24 hours, the sericin that will be adsorbed on activated carbon electrodes
It is parsed, parsing solution temperature is 65 DEG C, and the parsing time is 1.0h, then surveys obtained parsing solution with Kjeldahl's method
Sericin content in amount parsing solution obtains the sericin content in parsing solution as 4.3g, the rate of recovery 81.9%.
Embodiment does not form the limit to the scope of the present invention only to facilitate understand technical scheme of the present invention
System, any letter that every technical spirit without departing from technical solution of the present invention perhaps according to the present invention makees above scheme
Single modification, equivalent variations and modification, still fall within the scope of the present invention.
Embodiment 4
(1) property carbon powder is cleaned with deionized water to water conductivity and is down to 10us/cm, be subsequently placed in 100 DEG C of baking ovens
Drying, then by activated carbon, sodium carboxymethylcellulose, Kynoar according to 8:1:1 mass ratio mixing, then adds in quantitative
N-Methyl pyrrolidone makes it uniformly mix with magnetic stirrer 48h.Said mixture is coated in bubble using coating device
On foam nickel.The electrode of preparation is placed in baking oven and is dried.It is for use that activated carbon coating electrode finished product is made in last tabletting.
(2) cocoon boiling wastewater 1.5L micro-pore-film filtrations are taken, the solution after filtering is centrifuged to obtain supernatant and precipitation, are used
The NaOH solution of 1mol/L adjusts supernatant pH to 11, measures the sericin content in solution with Kjeldahl's method, obtains 1L
Protein content in supernatant is 5.25g, and sericin content is 0.21g in precipitation, so not considering sericin in precipitation
Content.
(3) using the activated carbon electrodes in step (1) as the cathode of electric adsorption device, expanded sheet metal is as electric adsorption device
Anode, supernatant 1L is taken in step (2) to carry out Electro Sorb adsorption time 48h, the sericin that will be adsorbed on activated carbon electrodes
It is parsed, parsing solution temperature is 95 DEG C, and the parsing time is 2.0h, then surveys obtained parsing solution with Kjeldahl's method
Sericin content in amount parsing solution obtains the sericin content in parsing solution as 3.9g, the rate of recovery 74.3%.
Embodiment does not form the limit to the scope of the present invention only to facilitate understand technical scheme of the present invention
System, any letter that every technical spirit without departing from technical solution of the present invention perhaps according to the present invention makees above scheme
Single modification, equivalent variations and modification, still fall within the scope of the present invention.
Claims (5)
1. a kind of embrane method processing cocoon boiling wastewater and the method for recycling sericin, which is characterized in that the recovery method include with
Lower step：
(1) preparation of activated carbon electrodes
Active carbon powder by 300 mesh molecular sieves is sieved, is then cleaned with deionized water to water conductivity and is down to 10~30 μ s/
Cm is subsequently placed in 90~120 DEG C of drying in oven, then activated carbon, sodium carboxymethylcellulose, Kynoar is mixed, then
N-Methyl pyrrolidone is added in, it is made uniformly to mix with 24~48h of magnetic stirrer；Using coating device by said mixture
Coated in nickel foam；The foam nickel electrode of preparation is placed in baking oven and is dried；Last tabletting be made activated carbon coating electrode into
Product are for use；
(2) sericin and wastewater treatment are recycled
Cocoon boiling wastewater first with microporous membrane filters is filtered, is centrifugally separating to obtain supernatant, activated carbon prepared by step (1) applies
Layer electrode is applied to electric adsorption device as electric anode as cathode, expanded sheet metal and carries out 24~48h of absorption, then by activated carbon
65 DEG C~85 DEG C of water or sodium hydroxide solution of sericin on electrode is parsed as desorbed solution, and the parsing time is
1.0~2.0h obtains sericin solution, and the sericin solution parsed is obtained by membrane distillation concentration, freeze-drying
Sericin powder；And the surplus solution after Electro Sorb is subjected to coagulating sedimentation, make the water quality discharge symbol of silk waste water after processing
Close wastewater discharge standard requirement.
2. a kind of embrane method processing cocoon boiling wastewater according to claim 1 and the method for recycling sericin, it is characterised in that：
Activated carbon, sodium carboxymethylcellulose, Kynoar mass mixing ratio be：8~10：1~2：1.
3. a kind of embrane method processing cocoon boiling wastewater according to claim 1 and the method for recycling sericin, it is characterised in that：
It is centrifugally separating to obtain supernatant and adjusts pH to 10~12.
4. a kind of embrane method processing cocoon boiling wastewater according to claim 1 and the method for recycling sericin, it is characterised in that：
Electric current is 0.05~2.0A, voltage 60V during the Electro Sorb.
5. a kind of embrane method processing cocoon boiling wastewater according to claim 1 and the method for recycling sericin, it is characterised in that：
The temperature control that desorbed solution is parsed is 80 DEG C~85 DEG C.
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