CN102584430B - Method for manufacturing amino-acid fishpond fertilizer water aqua by waste bave protein - Google Patents
Method for manufacturing amino-acid fishpond fertilizer water aqua by waste bave protein Download PDFInfo
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- CN102584430B CN102584430B CN2012100232692A CN201210023269A CN102584430B CN 102584430 B CN102584430 B CN 102584430B CN 2012100232692 A CN2012100232692 A CN 2012100232692A CN 201210023269 A CN201210023269 A CN 201210023269A CN 102584430 B CN102584430 B CN 102584430B
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Abstract
The invention relates to a method for manufacturing amino-acid fishpond fertilizer water aqua by waste bave protein. The method comprises the following steps of: preparing corresponding amino-acid hydrolysate by waste water, waste bave, waste silkworm pupae and the like of a reeling mill, and preparing the amino-acid fishpond fertilizer water aqua through the amino-acid hydrolysate, namely preparing amino-acid by hydrolyzing the bave protein, then adding urea, ammonium phosphate, potassium sulfate, ferric citrate, vitamin B1, vitamin B12, microbe consortium, trace elements and the like, and preparing the amino-acid fishpond fertilizer water aqua. According to the method, a brand-new way for reusing the reeling waste is developed, so that the cost and the pressure of the conventional sewage treatment method are reduced; and furthermore, the economic benefit of a factory and the yield of the factory are increased. The amino-acid fishpond fertilizer water aqua prepared by the method is low in cost, and has high quality and market competition. After the amino-acid fishpond fertilizer water aqua is added, the water quality can be improved effectively, so that the optimal growth environment is supplied to fishes.
Description
Technical field
The present invention relates to a kind of method of making fish pond rich water agent, particularly a kind of method of utilizing the fish pond rich water agent of discarded silk albumen manufacturing amino acid.
Background technology
The Guangxi located in subtropical zone has a moderate climate, and rainfall is abundant, very suitable freshwater fish culturing.Aqiuculrue is the main body of Guangxi fresh water fishery.Owing to be subjected to the restriction of geographical conditions, the water source that China has many places to breed fish leans on entirely or is most of by underground well water and natural river water.Fish pond water quality is thin, directly is used for breeding fish, and is unfavorable for the growth of fish.By using chemical fertilizer or fertilizer, the fish pond water quality of can fostering and apply fertilizer fast.The application for a patent for invention of Chinese patent application numbers 2009103063302.0 discloses a kind of rich water recombiner and preparation method thereof, and it is made up of photosynthetic bacterium, ammonium sulfate, calcium superphosphate and fertilizer.But use chemical fertilizer or fertilizer, may cause organic content superelevation in the pond, sink in the pool, bring water pollution and pathogenic micro-organism problem might for the pond culture system, the pond fish growth is caused have a strong impact on.
Under the industry policy of country " eastern Sang Xiyi " was guided, the Guangxi District Party Committee, government seized the opportunity, and transform agricultural production, and greatly develop the silkworm industry.Guangxi has become Chinese silk main producing region rapidly.Along with developing rapidly of Guangxi filature industry, the filature waste also rapidly increases.Governments at all levels also have to face the environmental improvement problem that the silk reeling wastewater waste is caused in the industry development of the local silk cocoon silk of promotion.Silk mill's waste mainly comprises: silk mill's waste water, discarded silk, discarded silkworm chrysalis etc.Silk reeling wastewater contains abundant sericine and pupal cell protein, belong to the organic wastewater of higher concentration, but biodegradability is good, safety non-toxic.Discarded silk, discarded silkworm chrysalis etc. contain rich in protein.The piques waste silk that produces in the silk reeling process is good protein source, is the high quality raw material of production fish pond amino acid fertilizer aqua.Therefore, make corresponding amino acid hydrolyticsolution if can effectively utilize silk mill's waste water, discarded silk, discarded silkworm chrysalis etc., and by the fish pond rich water agent of amino acid hydrolyticsolution making amino acid, not only can alleviate cost and pressure that traditional wastewater is handled, and can also open up the brand-new approach that a filature waste utilizes again conscientiously.
The amino acid fertilizer aqua is by multiple amino acids, nutritive salt, trace element, various active such as VITAMIN and enzymatic microorganism material and somatomedin, by activating the beneficial microorganism breeding and activating alga cells division and spore germination, promote unicellular algae (diatom and green alga) metabolism, coordinating algae balances each other with bacterium, impel water body rapidly fertile and keep water conditioning, enrich the water body natural bait, improve the fishes and shrimps seedling percent, promote the fishes and shrimps growth, effectively prevent from simultaneously to raise the nose above water to breathe or the general pool, reduce ammonia nitrogen in the water, nitrite, Toxic content such as hydrogen sulfide, reduce disease and take place, the amino acid fertilizer aqua product more and more is subjected to the popular welcome and the employing of various circles of society.But, because protein, particularly origin of amino acid is limited, therefore, tradition amino acid fertilizer aqua cost is higher, utilize the discarded albumen of filature to develop fish pond of high quality and at a reasonable price special-purpose amino acid rich water agent product, characteristics with super quality and competitive price, has the competitive edge that traditional amino acid fertilizer aqua product is lacked, present piques, waste silk, useless silkworm chrysalis etc., except having certain development and use, utilize the discarded protein Preparation amino acid fertilizer aqua product of filature not see as yet that both at home and abroad report is arranged at aspects such as silk flosssilk wadding, silk spinning, feeds.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of and utilize discarded silk albumen to make the method for amino acid fish pond rich water agent, this method has been opened up the brand-new approach that the filature waste utilizes again, not only can alleviate cost and pressure that traditional wastewater is handled, and improved the factory economy benefit, solved above-mentioned problems of the prior art.
The technical scheme that addresses the above problem is: a kind of method of utilizing the fish pond rich water agent of discarded silk albumen manufacturing amino acid may further comprise the steps:
(1) the discarded fibroin of filature reclaims: get filature basinetto silk sewage, with the saturated ammonium sulphate solution precipitation or with hydrochloric acid conditioning solution pH to the sericin iso-electric point, solution is removed in centrifugation, get to obtain crin albumen after precipitating vacuum concentration,
(2) utilize piques waste silk protein Preparation amino acid: get crin albumen that step (1) makes and mix with the piques waste silk and obtain mixture, NaOH solution hydrolysed mix with mass concentration 6～8%, the add-on ratio of mixture and NaOH solution is 1g:15～16ml, hydrolytic action time 15～20min, after hydrolysis finishes, with the hydrochloric acid neutralization, be 7～7.5 promptly again with hydrochloric acid conditioning solution pH value, obtain the silk protein hydrolyte, it is standby to obtain solid amino acid behind the vacuum concentration;
(3) utilize discarded pupa albumen to prepare amino acid: to add 5～10ml water by the discarded dried silkworm chrysalis meal of 1g, to discard the mixing of dried silkworm chrysalis meal and water pours in the reactor, regulating the pH value is 6～7, the papoid that adds discarded dried silkworm chrysalis meal quality 0.3～0.7% then, between 50 ℃～60 ℃, stir hydrolysis 7～9 hours, add 2～3mol/L hydrochloric acid soln again, the add-on of hydrochloric acid soln adds 1～2ml hydrochloric acid by the discarded dried silkworm chrysalis meal of 1g, between 100 ℃～110 ℃, stirred catalytic hydrolysis 7～9 hours, after hydrolysis finishes, neutralize with NaOH solution, be 7～7.5 with NaOH solution regulator solution pH value promptly, obtain the pupa albumen hydrolyzed solution, it is standby to obtain solid amino acid behind the vacuum concentration;
(4) preparation amino acid fish pond rich water agent: after the amino acid mixing that step (2) and step (3) are prepared, add aquatic benefit materials, adding entry again, to prepare amino acid whose mass content be 20%～30%, the mass content of aquatic benefit materials is 0.26%～0.52% amino acid fish pond rich water agent, and described aquatic benefit materials is urea, ammonium phosphate, vitriolate of tartar, ironic citrate, VITMAIN B1, vitamin B12, microorganism species and contains microelement substance.
Rich water agent mass content in described amino acid fish pond is: amino acid 20%～30%, urea 0.1～0.2%, ammonium phosphate 0.1～0.2%, vitriolate of tartar 0.01～0.02%, ironic citrate 0.01～0.02%, VITMAIN B1 and vitamin B12 each 0.01～0.02%, microorganism species 0.01%～0.02%, contain microelement substance 0.01～0.02%, surplus is a sterilized water, the solid quality content of this amino acid fish pond rich water agent is lower than 40%.
Described microorganism species is bacillus megaterium, Rhodopseudomonas palustris or vinelandii.
The described microelement substance that contains is meant soil extract.
Further technical scheme of the present invention is: in the described step (1), after obtaining crin albumen behind the vacuum concentration, after again crin albumen being put into petroleum ether solution and being soaked degreasing in 22～26 hours, filter, get filtrate and carry out the crin albumen that obtains being further purified after the lyophilize, again crin albumen is mixed into mixture with the piques waste silk in step (2).
Described vacuum concentration be-0.093 at pressure～-0.098Mpa, temperature are to carry out under 70～75 ℃ of conditions, till being concentrated into solution and having crystallization to separate out.
Further technical scheme of the present invention is: in the step (1), get filature basinetto silk sewage, transfer to full state of saturation with ammonium sulfate, discarded silk albumen precipitation is separated out.
Another further technical scheme of the present invention is: in the step (1), get filature basinetto silk sewage, to the sericin iso-electric point, promptly use hydrochloric acid conditioning solution PH3.8～4.4 with hydrochloric acid conditioning solution pH.
Amino acid whose mass content 〉=90.5% in the solid amino acid that obtains behind step (2) and step (3) vacuum concentration.
Compared with prior art, the present invention a kind of utilize discarded silk albumen make amino acid fish pond rich water agent method have a following beneficial effect:
1. open up the brand-new approach that the filature waste utilizes again, not only can alleviate cost and pressure that traditional wastewater is handled, and improve the factory economy benefit, increased factory's output value.
The present invention designs production fish pond amino acid fertilizer aqua with silk mill's waste for main raw material, and silk mill's waste mainly comprises: silk mill's waste water, discarded silk, discarded silkworm chrysalis etc.The present invention recycles silk mill's waste water (basinetto silk sewage), discarded silk and discarded silkworm chrysalis, makes corresponding amino acid hydrolyticsolution by hydrolysis method, after the vacuum concentration removal of impurities, obtains the amino acid of content 〉=90.5%.With this amino acid is main raw material, adds the essential element and the aquatic probiotics of multiple algal grown, prepares a seed amino acid fish pond rich water agent.When solving silk mill's problem of environmental pollution, rationally utilize the filature byproduct, turn waste into wealth, conscientiously opened up a brand-new approach that the filature waste utilizes again, not only can alleviate cost and pressure that traditional wastewater is handled, and can also improve the factory economy benefit, increase factory's output value.
2. the amino acid fertilizer aqua that adopts the inventive method to prepare, cost is low, and super quality and competitive price have the market competitiveness.
Silk reeling wastewater contains abundant sericine and pupal cell protein, belong to the organic wastewater of higher concentration, but biodegradability is good, safety non-toxic.Discarded silk, discarded silkworm chrysalis etc. contain rich in protein.So the piques waste silk that produces in the silk reeling process is good protein source, is the high quality raw material of production fish pond amino acid fertilizer aqua.Preparation technology of the present invention is simple, for example utilizes discarded pupa albumen to prepare in the amino acid step, and hydrolysis time shortens greatly than traditional hydrolysis process, and degree of hydrolysis reaches 98.17%.Owing to be that the employing waste is a raw material, the rich water agent cost of the present invention's preparation is low in addition, and super quality and competitive price have the competitive edge that traditional amino acid fertilizer aqua product is lacked.
3. the amino acid fertilizer aqua that adopts the inventive method to prepare can improve the growing environment of fish, promotes fish growth, improves fish pond output.
The present invention utilizes the useless silkworm chrysalis of filature byproduct piques waste silk to prepare amino acid, does not use the fertilizer component, and has added multiple aquatic benefit materials, VITAMIN, bacillus megaterium, Rhodopseudomonas palustris, vinelandii etc.Wherein the interpolation of VITAMIN can improve algae grows rate and survival rate, and the interpolation of bacillus megaterium, Rhodopseudomonas palustris and vinelandii can increase dissolved oxygen in water by id reaction, reduces H in the water
2S and free N, P content, organism in the water of decomposition greatly for the vegeto-animal growth of swimming provides small molecules nutriment, purifies water again, improves the fish growth environment, promotes fish growth, and then reaches the final purpose that improves output.
Below, a kind of technical characterictic that utilizes discarded silk albumen to make the method for amino acid fish pond rich water agent to the present invention is further described in conjunction with the accompanying drawings and embodiments.
Description of drawings
Fig. 1: a kind of of the present invention utilizes discarded silk albumen to make the method process flow sheet of amino acid fish pond rich water agent.
Embodiment
A kind of method of utilizing the fish pond rich water agent of discarded silk albumen manufacturing amino acid may further comprise the steps:
(1) the discarded fibroin of filature reclaims: get filature basinetto silk sewage, with hydrochloric acid conditioning solution pH to the sericin iso-electric point, promptly use hydrochloric acid conditioning solution PH3.8～4.4, centrifugation 30min, remove solution, obtain crin albumen after getting the precipitation vacuum concentration, after putting into petroleum ether solution and soaking degreasing in 24 hours, filter, get filtrate and carry out the crin albumen that obtains being further purified after the lyophilize.
(2) utilize piques waste silk protein Preparation amino acid: get crin albumen that step (1) makes and mix with the piques waste silk and obtain mixture, NaOH solution hydrolysed mix with mass concentration 7%, the add-on ratio of mixture and NaOH solution is 1g:15.2ml, hydrolytic action time 16min, after hydrolysis finishes, with the hydrochloric acid neutralization, be 7～7.5 promptly again with hydrochloric acid conditioning solution pH value, obtain the silk protein hydrolyte, it is standby to obtain solid amino acid behind the vacuum concentration.
(3) utilize discarded pupa albumen to prepare amino acid: to add 7ml water by the discarded dried silkworm chrysalis meal of 1g, to discard the mixing of dried silkworm chrysalis meal and water pours in the reactor, regulating the pH value is 6.5, the papoid that adds discarded dried silkworm chrysalis meal quality 0.5% then, between 50 ℃～60 ℃, stir hydrolysis 8 hours, add the 3mol/L hydrochloric acid soln again, the add-on of hydrochloric acid soln adds 1～2ml hydrochloric acid by the discarded dried silkworm chrysalis meal of 1g, between 100 ℃～110 ℃, stirred catalytic hydrolysis 8 hours, after hydrolysis finishes, neutralize with NaOH solution, be 7～7.5 with NaOH solution regulator solution pH value promptly, obtain the pupa albumen hydrolyzed solution, it is standby to obtain solid amino acid behind the vacuum concentration.
(4) preparation amino acid fish pond rich water agent: after the amino acid mixing that step (2) and step (3) are prepared, add aquatic benefit materials, add entry again and prepare the rich water agent of amino acid fish pond, rich water agent mass content in described amino acid fish pond is: amino acid 20%～30%, urea 0.1～0.2%, ammonium phosphate 0.1～0.2%, vitriolate of tartar 0.01～0.02%, ironic citrate 0.01～0.02%, VITMAIN B1 and vitamin B12 each 0.01～0.02%, microorganism species 0.01%～0.02%, soil extract 0.01～0.02%, surplus is a sterilized water, and the solid quality content of this amino acid fish pond rich water agent is lower than 40%.
Microorganism species of the present invention is bacillus megaterium, Rhodopseudomonas palustris or vinelandii.Described soil extract is meant that the fertile soil that takes out from places such as fish pond, rice terraces adds 1ml water by 1g soil and adds the water stirring, filters the resulting liquid in back and is soil extract.Mainly contain trace element in the soil extract, as a kind of conversion of present embodiment, also available commercially available trace element replaces soil extract.
Vacuum concentration of the present invention generally be-0.093 at pressure～-0.098Mpa, temperature are to carry out under 70～75 ℃ of conditions, till being concentrated into solution and having crystallization to separate out, amino acid whose mass content 〉=90.5% in the solid amino acid that obtains behind step (2) and step (3) vacuum concentration.
A kind of conversion as present embodiment, during the discarded fibroin of described step (1) filature reclaims, get filature basinetto silk sewage, except using hydrochloric acid conditioning solution pH to the sericin iso-electric point, can also transfer to full state of saturation with ammonium sulfate, discarded silk albumen precipitation is separated out, and solution is removed in centrifugation, obtains crin albumen after getting the precipitation vacuum concentration.
Another conversion as present embodiment, in the step (1), centrifugation, after obtaining crin albumen behind the precipitation vacuum concentration, can directly crin albumen be mixed with the piques waste silk and carry out step (2), can in the cancellation step (1) crin albumen be put into petroleum ether solution soak degreasing, filtration, cryodesiccated operation.
Another conversion as present embodiment, the ratio of each component in the aquatic benefit materials in the rich water agent of described amino acid fish pond, be that urea, ammonium phosphate, vitriolate of tartar, ironic citrate, VITMAIN B1, vitamin B12, microorganism species and the adding proportion that contains microelement substance can also be according to the practical situation adjustment, amino acid whose mass content is 20%～30% in the rich water agent of amino acid fish pond as long as satisfy, and the mass content of aquatic benefit materials is that 0.26%～0.52% condition gets final product.
Solid content of the present invention is meant that ordinary method evaporation (promptly under normal pressure, vaporization temperature is 100 ℃) drained weight that obtains accounts for the ratio of total solution weight.
The amino acid fish pond rich water agent that the present invention prepares contains the suitableeest nutritional factor that is suitable for unicellular green algate of fresh water class growth and the microorganism species that improves water quality.In the fish pond,, on the one hand,, can effectively improve water quality, reduce H in the water by its algae and beneficial microorganism by adding product of the present invention
2S and free N, P content, decomposing organic compounds for fish growth provides best growing environment, on the other hand, also is a kind of environmental friendliness treatment process of efficient processing filature waste.
Claims (6)
1. one kind is utilized discarded silk albumen to make the method for amino acid fish pond rich water agent, it is characterized in that: may further comprise the steps:
(1) the discarded fibroin of filature reclaims: get filature basinetto silk sewage, with the saturated ammonium sulphate solution precipitation or with hydrochloric acid conditioning solution pH to the sericin iso-electric point, solution is removed in centrifugation, gets to obtain crin albumen after precipitating vacuum concentration;
(2) utilize piques waste silk protein Preparation amino acid: get crin albumen that step (1) makes and mix with the piques waste silk and obtain mixture, NaOH solution hydrolysed mix with mass concentration 6～8%, the add-on ratio of mixture and NaOH solution is 1g:15～16ml, hydrolytic action time 15～20min, after hydrolysis finishes, with the hydrochloric acid neutralization, be 7～7.5 promptly again with hydrochloric acid conditioning solution pH value, obtain the silk protein hydrolyte, it is standby to obtain solid amino acid behind the vacuum concentration;
(3) utilize discarded pupa albumen to prepare amino acid: to add 5～10ml water by the discarded dried silkworm chrysalis meal of 1g, to discard the mixing of dried silkworm chrysalis meal and water pours in the reactor, regulating the pH value is 6～7, the papoid that adds discarded dried silkworm chrysalis meal quality 0.3～0.7% then, between 50 ℃～60 ℃, stir hydrolysis 7～9 hours, add 2～3mol/L hydrochloric acid soln again, the add-on of hydrochloric acid soln adds 1～2ml hydrochloric acid by the discarded dried silkworm chrysalis meal of 1g, between 100 ℃～110 ℃, stirred catalytic hydrolysis 7～9 hours, after hydrolysis finishes, neutralize with NaOH solution, be 7～7.5 with NaOH solution regulator solution pH value promptly, obtain the pupa albumen hydrolyzed solution, it is standby to obtain solid amino acid behind the vacuum concentration;
(4) preparation amino acid fish pond rich water agent: after the amino acid mixing that step (2) and step (3) are prepared, add aquatic benefit materials, adding entry again, to prepare amino acid whose mass content be 20%～30%, the mass content of aquatic benefit materials is 0.26%～0.52% amino acid fish pond rich water agent, and described aquatic benefit materials is urea, ammonium phosphate, vitriolate of tartar, ironic citrate, VITMAIN B1, vitamin B12, microorganism species and contains microelement substance; The described microelement substance that contains is meant soil extract, and the fertile soil that described soil extract is meant from the fish pond, rice terrace takes out adds 1ml water by 1g soil and adds the water stirring, filters the resulting liquid in back;
Vacuum concentration described in step (1), (2) and (3) be-0.093 at pressure～-0.098Mpa, temperature are to carry out under 70～75 ℃ of conditions, till being concentrated into solution and having crystallization to separate out;
The described amino acid fish pond rich water agent mass content for preparing is: amino acid 20%～30%, urea 0.1～0.2%, ammonium phosphate 0.1～0.2%, vitriolate of tartar 0.01～0.02%, ironic citrate 0.01～0.02%, VITMAIN B1 and vitamin B12 each 0.01～0.02%, microorganism species 0.01%～0.02%, contain microelement substance 0.01～0.02%, surplus is a sterilized water, the solid quality content of this amino acid fish pond rich water agent is lower than 40%.
2. a kind of method of utilizing the fish pond rich water agent of discarded silk albumen manufacturing amino acid according to claim 1, it is characterized in that: described microorganism species is bacillus megaterium, Rhodopseudomonas palustris or vinelandii.
3. a kind of method of utilizing the fish pond rich water agent of discarded silk albumen manufacturing amino acid according to claim 1 and 2, it is characterized in that: in the described step (1), after obtaining crin albumen behind the vacuum concentration, after again crin albumen being put into petroleum ether solution and being soaked degreasing in 22～26 hours, filter, get filtrate and carry out the crin albumen that obtains being further purified after the lyophilize, again crin albumen is mixed into mixture with the piques waste silk in step (2).
4. a kind of method of utilizing the fish pond rich water agent of discarded silk albumen manufacturing amino acid according to claim 1 and 2, it is characterized in that: in the step (1), get filature basinetto silk sewage, transfer to full state of saturation, discarded silk albumen precipitation is separated out with ammonium sulfate.
5. a kind of method of utilizing the fish pond rich water agent of discarded silk albumen manufacturing amino acid according to claim 1 and 2, it is characterized in that: in the step (1), get filature basinetto silk sewage, to the sericin iso-electric point, promptly use hydrochloric acid conditioning solution pH3.8～4.4 with hydrochloric acid conditioning solution pH.
6. a kind of method of utilizing the fish pond rich water agent of discarded silk albumen manufacturing amino acid according to claim 1 and 2 is characterized in that: amino acid whose mass content 〉=90.5% in the solid amino acid that obtains behind step (2) and step (3) vacuum concentration.
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| CN104058877B (en) * | 2014-07-14 | 2016-03-02 | 丹东中天柞蚕生物科技有限公司 | Sericin biological organic complex fertilizer and method for making |
| CN104058876B (en) * | 2014-07-14 | 2016-02-03 | 丹东中天柞蚕生物科技有限公司 | Sericin multiple-effect liquid bio-organic fertilizer and method for making |
| CN106032346A (en) * | 2015-07-08 | 2016-10-19 | 魏滔 | Method for treating filature factory waste water |
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| CN106804892A (en) * | 2017-01-26 | 2017-06-09 | 黔东南贵人蚕业开发有限公司 | A kind of method that silkworm chrysalis protein is extracted from fresh silk cocoon silk reeling wastewater |
| CN108484266A (en) * | 2018-04-21 | 2018-09-04 | 重庆尚奕辉生物科技有限公司 | A kind of production method of liquid compound fertilizer and its use and methods for using them |
| CN111280309A (en) * | 2020-03-13 | 2020-06-16 | 易维杰 | Sericin trace element compound and preparation method and application thereof |
| DE102021131918A1 (en) * | 2021-12-03 | 2023-06-07 | Fibrothelium Gmbh | Process for producing at least one fibroin solution |
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