CN105284882B - A kind of oyster shell stealth chlorine dioxide anti-biotic material and preparation method thereof and application method - Google Patents
A kind of oyster shell stealth chlorine dioxide anti-biotic material and preparation method thereof and application method Download PDFInfo
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Abstract
The invention discloses a kind of oyster shell stealth chlorine dioxide anti-biotic material and preparation method thereof and application method, its oyster shell stealth chlorine dioxide anti-biotic material, the oyster shell powder for being particle diameter below 50 μm and sodium chlorite powder, the mixture of niter cake powder, the weight ratio of three is the ︰ 0.1 0.2 of 1 ︰ 0.05 0.1；Wherein, the oyster shell powder has loose and porous structure, is using oyster shell as raw material, through calcining, grinding, obtained high activity powder.Clinker is made by three-level staged heating calcination method in its preparation method, has loose and porous structure and high chemism to obtain；The application method of its Practice for Pesticide Residue in Agricultural Products that is used to dispelling is simple, safe and efficient, non-secondary pollution is without generation.The present invention has the characteristics that low cost, energy-conserving and environment-protective, safe to use, efficient, green relative to prior art, and the washing suitable for all kinds of fruits and vegetables is handled, and can effectively dispel the farm chemical ingredients residual of attachment in its surface, and broad-spectrum sterilization.
Description
Technical field
The present invention relates to a kind of anti-biotic material and preparation method thereof and its application method, more particularly to a kind of oyster shell-hidden
The application method of shape chlorine dioxide anti-biotic material and preparation method thereof and its Practice for Pesticide Residue in Agricultural Products of dispelling, belong to oyster shell and be modified skill
Art field.
Background technology
China's seashells kind class is a lot, and 2014 annual productions reach 14,000,000 tons.Wherein, oyster yield is maximum, produces per year
Amount reaches 4,100,000 tons.The shell of oyster, which weighs about, accounts for more than the 75% of oyster gross weight.That is, China will produce about 3,000,000 every year
Oyster shell more than ton.
Oyster shell solid waste, if being discarded into natural environment, the attractive in appearance of environment can not only be had a negative impact,
And substantial amounts of usable land is taken, while also because it gives out dense fish-stench, and influence urban air-quality and people
Life.
2007, Kanazawa, Japan Security at sea portion assert that oyster shell is waste items, thus has issued and forbidden arbitrarily toppling over
Ban, forbid arbitrarily putting into oyster shell it is marine, to avoid its pollution of marine environment.
In recent years, carried out in terms of how people are for carry out the harmless treatment of oyster shell and its recycling of resource
Largely benefit our pursuits and study, and achieve a series of technological progress, be harmless treatment and its resource of oyster shell
Recycling hews out a variety of practical application approaches.Such as：
Chinese patent application CN103087851B discloses degerming cleaning agent of a kind of vegetables, melon and fruit and preparation method thereof, its
Mixed by the shell for by parts by weight being respectively oyster shell 2-4 parts, variegated clam shell 3-5 parts and scallop shell 2-4 parts, through 800-
1600 DEG C of burning 7-9 hours, add after accounting for material gross weight 18-22% water reaction, through 280-320 DEG C of drying；It will pass through again
Material after drying burns 5-7 hours at 950-1050 DEG C；Then, the material that burning finishes is produced into powder through high microcomputer
Afterwards, it is well mixed with accounting for material gross weight 7-9% activated carbon and accounting for material gross weight 4-6% chitin, vegetables, melon is made
The degerming cleaning agent of fruit.
But above-mentioned technical proposal is on the one hand, the oyster shell whiting that calcining heat is high, energy resource consumption is greatly, after calcining be present and live
Property is relatively low, porosity is also not high enough；On the other hand, it needs to add the activated carbon for accounting for material gross weight 7-9% and to account for material total
Weight 4-6% chitin, this is cause its production cost further up, and the vegetable after its immersion, leaching drift
Dish, melon and fruit are also needed to after being rinsed well using substantial amounts of clear water, could meet safe edible requirement.
The content of the invention
It is an object of the invention to provide a kind of short texture is porous, active sufficiently high, the low oyster shell of production cost
Powder, and based on it raw material be used for dispel crop products and fruit residues of pesticides oyster shell-stealthy chlorine dioxide
Anti-biotic material.
The technical issues that need to address are how effectively to reduce production cost, utilize this to the present invention to achieve the above object
Oyster shell powder, prepare suitable for fruit, the cleaning of greengrocery primary agricultural products, asked with dispelling the technology of its residues of pesticides composition
Topic.
The present invention is to achieve the above object the technical scheme adopted is that a kind of oyster shell-stealthy chlorine dioxide antibacterial material
Material, it is characterised in that for oyster shell powder of the particle diameter below 50 μm and sodium chlorite, the mixture of niter cake powder, institute
The weight ratio for stating oyster shell powder, sodium chlorite and niter cake powder in mixture is 1 ︰ 0.05-0.1 ︰ 0.1-0.2；
The oyster shell powder has loose and porous structure, is using cheap solid waste biological material oyster shell as original
Material, through calcining, grinding, obtained active powder.
The technical effect directly brought by the technical proposal is that oyster shell-stealthy chlorine dioxide anti-biotic material is produced into
This is low, without poisonous and harmful chemical composition, and suitable for the washing of all kinds of water fruits and vegetables primary agricultural products, its surface is attached to dispel
On residues of pesticides composition, and can effectively kill the Escherichia coli on its surface, its is safe to use, efficient, useless after use
Liquid/waste water is nontoxic pollution-free.
That is, the oyster shell of above-mentioned technical proposal-stealthy chlorine dioxide anti-biotic material for it is safe efficient, green just
The washing product of level agricultural product.
In above-mentioned technical proposal, in the oyster shell powder of loose and porous structure, it is aided with stealthy chlorine dioxide raw material Asia chlorine
Sour sodium, niter cake, strength oxidant can be produced in the application：Chlorine dioxide.
To more fully understand this technical characterstic, now describe in detail as follows：
10NaClO2+8NaHSO4=8ClO2↑+5Na2SO4+4H2O
Chlorine dioxide environmentally friendly material recognized in the world.
The ostreae testa pulverata of loose and porous structure will produce as follows with stealthy chlorine dioxide raw material sodium chlorite, niter cake collocation
Special-effect：
(1) generally, sodium chlorite and niter cake be can not the taboo of independent mixed storage arrange in pairs or groups property material；Loose structure
Ostreae testa pulverata is arranged in pairs or groups with both, both is protected respectively, is served inertia protective effect, can be deposited for a long time anti-without occurring
Should.
(2) the defects of stealth technique overcomes Chlorine Dioxide Gas inconvenience storage, transport, used, it is only when in use
Chlorine dioxide can be just discharged, both safety, and practical.
(3) chlorine dioxide is the green of highest level recognized in the world, high-effective disinfecting, bactericide, have efficiently, it is wide
Spectrum, the advantages that dosage is few, quick, the duration is long, nontoxic.It to Pseudomonas aeruginosa, Escherichia coli, tubercle bacillus, typhoid bacillus,
Bacillus, bacteriophage, hcrpesviruses, hepatitis B, encephalomyelitis virus, SARS virus, etc. killing rate be up to
100%.It coordinates not with loose and porous structure ostreae testa pulverata only has the clean effect of strong disinfecting, and loose structure ostreae testa pulverata can be inhaled
Attached chlorine dioxide, increases chlorine dioxide slow-release, and effect is more longlasting；Its volatility is reduced simultaneously, prevents local environment two
Chlorine monoxid concentration over-standard (is more than 3mg/m3) operator is damaged.
(4) chlorine dioxide can eliminate formaldehyde, benzene, ammonia, hydrogen sulfide noxious material.For example, can efficiently oxidation of formaldehyde into
Carbon dioxide and water innocuous substance.Especially can be common are machine phosphorus or carbamate chemicals for agriculture oxidation, so as to destroy it
Structure, it is changed into small molecule, its toxicity of degrading.The ostreae testa pulverata of chlorine dioxide and loose and porous structure coordinates, loose and porous structure
Ostreae testa pulverata adsorbs the slow release of chlorine dioxide so that the toxicity reduction effect of chlorine dioxide is more lasting, and effect is more preferable.I.e. so that sub-
Both sodium chlorate and niter cake can arrange in pairs or groups use, and produce obvious cooperative effect.
The second object of the present invention is to provide a kind of preparation side of above-mentioned oyster shell-stealthy chlorine dioxide anti-biotic material
Method.
The present invention reduces energy consumption, and obtain to realize the purpose technical issues that need to address are how to improve calcine technology
Obtain the technical problem of porous, the active sufficiently high oyster shell powder of short texture.
The present invention is in order to solve the above technical problems, the technical scheme used is a kind of above-mentioned oyster shell-stealthy titanium dioxide
The preparation method of chlorine anti-biotic material, it is characterised in that comprise the following steps：
The first step, first the oyster shell for banking up spontaneous fermentation purification is first cleaned up with clear water, again through drying or in nature
Dried in the shade under ventilation condition, after be crushed to particle diameter be 0.5-3.5mm particle, raw material are made；
Second step, above-mentioned raw material are entered into high temperature furnace, clinker is made using three-level staged heating calcination method；Specific calcining step
It is rapid as follows：
After being first warming up to 300-350 DEG C with 2 DEG C/min of heating rate, 10min is incubated；
Then, after being continuously heating to 650 DEG C with 5 DEG C/min of heating rate, 15-20min is incubated, it is then, aeration-cooling
To 600 DEG C；
After being warming up to 810-830 DEG C again with 10 DEG C/min of heating rate, 20-40min is incubated；Then, it is aeration-cooling extremely
750 DEG C, and 20min is incubated, produce clinker；
3rd step, clinker take out after naturally cooling to room temperature；By the clinker after cooling enter grinding machine grinding into particle diameter be 50 μ
Below m powder；
By it is above-mentioned by powder made from grinding and sodium chlorite powder, niter cake powder weight than 1 ︰ 0.05-
0.1 ︰ 0.1-0.2 are well mixed, and are produced.
The technical effect directly brought by the technical proposal is that calcining heat is low, when, its production process more saves；
What is more important, (oyster shell) clinker for calcining gained have excellent chemism, also, loose porous in its structure,
Specific surface area is bigger, bulk density is smaller, thus has very excellent surface adsorption property.
The third object of the present invention is to provide a kind of above-mentioned oyster shell-stealthy chlorine dioxide anti-biotic material and dispelled agricultural product
The application method of residues of pesticides.
The present invention is to realize the purpose the technical scheme adopted is that a kind of above-mentioned oyster shell-stealthy chlorine dioxide resists
Bacterium material is dispelled the application method of Practice for Pesticide Residue in Agricultural Products, it is characterised in that the agricultural product are fruit, greengrocery primary agricultural production
Product, the application method comprise the following steps：
The first step, oyster shell-stealthy chlorine dioxide anti-biotic material is pressed 1:500-1000 mass ratio is dissolved in water, stirred
It is even, it is configured to water for cleaning solution；
Second step, fruit, greengrocery primary agricultural products are immersed in above-mentioned water for cleaning solution, soak 10-15min；
3rd step, fruit, greengrocery primary agricultural products are pulled out, and rinsed well with a small amount of clear water, is attached to removing
The remaining oyster shell on its surface-stealthy chlorine dioxide anti-biotic material, can be with the food materials of safe edible.
The technical effect directly brought by the technical proposal is that application method is simple, non-secondary pollution thing produces；
Also, its use cost is low：First, water for cleaning solution is by oyster shell powder anti-biotic material and water 1:500-1000
Mass ratio directly dilute preparation；Second, because oyster shell powder anti-biotic material is without any poisonous and harmful chemical composition, itself
The basic demand of safe edible can fully be met, thus, after being soaked by this oyster shell powder anti-biotic material, dispel
Except residues of pesticides and the fruits and vegetables of killing bacteria, it is not necessary to reuse excessive clear water and be rinsed.That is, using process
In, more economize on water, safety.
In summary, the present invention is heated using three step ladder-elevating temperatures and is calcined using natural oyster shell solid waste as raw material,
With reference to the calcine technology of ventilation method, the ostreae testa pulverata of special structure form for having that short texture is porous, chemism is high is obtained, then
It is aided with food-grade stealth chlorine dioxide powder, the removal of all kinds of vegetables or all kinds of fruit surface residues of pesticides can be directly used in, with
And the functional material of sterilizing and harmful bacteria.
The present invention has the advantages that relative to prior art：
1st, be raw material using cheap natural oyster shell, obtain not only with prior art artificial synthetic organic materials or inorganic
The identical even more preferable washing effect of vegetables prepared by the compound of oxidant and surfactant, melon and fruit liquid detergent, moreover it is possible to
Remove residues of pesticides and harmful bacteria, no Secondary Organic thing, antibiotic residue are natural, non-polluted edible security is more preferable；
2nd, decontamination degerming functions material prepared by single oyster shell material, than use and scallop shell, variegated clam shell or mix
Shell material removes residues of pesticides and the effect of harmful bacteria is more preferable；
3rd, three steps ladder heating roasting ventilation method can not only make oyster have porous material structure, and absorption property is good, and
Inert gas shielding is not required to, sintering temperature is relatively low, and cost is lower, belongs to green energy conservation technical process.
4th, in the oyster powder of loose and porous structure, it is aided with stealthy chlorine dioxide raw material sodium chlorite, niter cake, profit
Broad-spectrum sterilization is carried out with caused strength oxidant chlorine dioxide during its use, and dexterously utilizes loose and porous structure
Absorption of the oyster to chlorine dioxide, to increase chlorine dioxide slow-release so that its effect is more longlasting；Simultaneously it is reduced to wave
Hair property, prevents local environment chlorine dioxide concentration is exceeded (to be more than 3mg/m3) operator is damaged.I.e. so that chlorine dioxide
Toxicity reduction effect it is more lasting, effect is more preferable.
Brief description of the drawings
Fig. 1 is Bactericidal test of the oyster shell-stealthy chlorine dioxide anti-biotic material obtained by embodiment 1 to Escherichia coli
As a result.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
Oyster shell-stealthy chlorine dioxide anti-biotic material is prepared as follows：
The first step, first the oyster shell for banking up spontaneous fermentation purification is first cleaned up with clear water, again through drying or in nature
Dried in the shade under ventilation condition, after be crushed to particle diameter be 0.5-2.5mm particle, raw material are made；
Second step, above-mentioned raw material are entered into high temperature furnace, clinker is made using three-level staged heating calcination method；Specific calcining step
It is rapid as follows：
After being first warming up to 300 DEG C with 2 DEG C/min of heating rate, 10min is incubated；
Then, after being continuously heating to 650 DEG C with 5 DEG C/min of heating rate, it is incubated 15min；Then, it is aeration-cooling extremely
600℃；
After being warming up to 810 DEG C again with 10 DEG C/min of heating rate, 40min is incubated；Then, aeration-cooling to 750 DEG C,
And 20min is incubated, produce clinker；
3rd step, clinker take out after naturally cooling to room temperature；By the clinker after cooling enter grinding machine grinding into particle diameter be 50 μ
Below m, obtain oyster shell powder；
Above-mentioned oyster shell powder is mixed with sodium chlorite powder, niter cake powder by weight the ︰ 0.1 of 1 ︰ 0.05
It is even, produce.
Embodiment 2
Oyster shell-stealthy chlorine dioxide anti-biotic material is prepared as follows：
The first step, first the oyster shell for banking up spontaneous fermentation purification is first cleaned up with clear water, again through drying or in nature
Dried in the shade under ventilation condition, after be crushed to particle diameter be 2.5-3.5mm particle, raw material are made；
Second step, above-mentioned raw material are entered into high temperature furnace, clinker is made using three-level staged heating calcination method；Specific calcining step
It is rapid as follows：
After being first warming up to 350 DEG C with 2 DEG C/min of heating rate, 10min is incubated；
Then, after being continuously heating to 650 DEG C with 5 DEG C/min of heating rate, it is incubated 20min；Then, it is aeration-cooling extremely
600℃；
After being warming up to 830 DEG C again with 10 DEG C/min of heating rate, 20min is incubated；Then, aeration-cooling to 750 DEG C,
And 20min is incubated, produce clinker；
3rd step, clinker take out after naturally cooling to room temperature；By the clinker after cooling enter grinding machine grinding into particle diameter be 20-
30 μm, obtain oyster shell powder；
Above-mentioned oyster shell powder is well mixed with sodium chlorite powder, niter cake powder by weight the ︰ 0.2 of 1 ︰ 0.1,
Produce.
Embodiment 3
Oyster shell-stealthy chlorine dioxide anti-biotic material is prepared as follows：
The first step, first the oyster shell for banking up spontaneous fermentation purification is first cleaned up with clear water, again through drying or in nature
Dried in the shade under ventilation condition, after be crushed to particle diameter be 0.5-3.5mm particle, raw material are made；
Second step, above-mentioned raw material are entered into high temperature furnace, clinker is made using three-level staged heating calcination method；Specific calcining step
It is rapid as follows：
After being first warming up to 330 DEG C with 2 DEG C/min of heating rate, 10min is incubated；
Then, after being continuously heating to 650 DEG C with 5 DEG C/min of heating rate, it is incubated 20min；Then, it is aeration-cooling extremely
600℃；
After being warming up to 820 DEG C again with 10 DEG C/min of heating rate, 30min is incubated；Then, aeration-cooling to 750 DEG C,
And 20min is incubated, produce clinker；
3rd step, clinker take out after naturally cooling to room temperature；By the clinker after cooling enter grinding machine grinding into particle diameter be 50 μ
Below m, obtain oyster shell powder；
Above-mentioned oyster shell powder is mixed with sodium chlorite powder, niter cake powder by weight the ︰ 0.15 of 1 ︰ 0.08
It is even, produce.
Choose embodiment 1 and be used as representative embodiment, the oyster shell obtained by it-stealthy chlorine dioxide anti-biotic material is produced
Product carry out test experience.The experimental method and testing result of detection are as follows：
(1) fruits and vegetables are put into the emulsion of flolimat containing agricultural chemicals 100mgL/L water to soak to pull out for 3 seconds and dried.
(2) product is put into water in the ratio of 5g/kg water and stirred evenly, be thereafter put into fruit and vegetable food, allow water just to cover
Fruits and vegetables, stir 2 times in 10min, pull out and drain, using clear water as contrast experiment；
(3) method of testing and instrument：Using LS-SC-32 rapid detector for pesticide residue (instrument traits：Using enzyme level
Rate method, meets standard GB/T/T5009.199-2003, persticide residue that can be in quick detection fruits and vegetables sample, Monitoring lower-cut
0.2ppm), with colour developing colorimetric method come test sample residual oxidization Rogor concentration.
Calculation formula：Absorbance A is tested under 412nm wavelength, persticide residue is represented with inhibiting rate, is calculated as follows：
S%=[(△ A0- △ At)/△ A0] × 100
In formula：S%--- inhibiting rates；
△ A0--- contrast solutions react the changing value of 3min absorbances；
△ At--- sample solutions react the changing value of 3min absorbances.
Persticide residue is with inhibiting rate criterion (standard GB/T/T5009.199-2003)：
| The inhibiting rate of fruits and vegetables sample | Fruit-vegetable quality | Evaluation and recommendations |
| 0%<Inhibiting rate<15% | Pollution-free vegetable | Outlet can be trusted |
| 15%<Inhibiting rate<30% | Green vegetables | Can be with safe edible |
| 30%<Inhibiting rate<50% | Pollution-free vegetable | Can be with safe edible |
| 50%<Inhibiting rate<100% | There are pollution by pesticides vegetables | It is unable to safe edible |
Testing result such as table 1 below：
Table 1
| Fruits and vegetables species | Product design (g/kg water) | Inhibiting rate (%) | Escherichia coli detect strain number | Conclusion |
| Clear water contrast experiment | Cucumber | 0 | 79 | 56 | It is exceeded |
| The present invention | Cucumber | 5 | 9 | 0 | It is qualified |
| The present invention | Cauliflower | 5 | 13 | 0 | It is qualified |
| The present invention | Rape | 5 | 14 | 0 | It is qualified |
| The present invention | Apple | 5 | 7 | 0 | It is qualified |
| The present invention | Strawberry | 5 | 12 | 0 | It is qualified |
Choose oyster shell-stealthy chlorine dioxide antibacterial material product obtained by embodiment 2 and carry out test experience.Detection
Experimental method is identical with the test experience method of embodiment 1, testing result such as table 2 below：
Table 2
| Fruits and vegetables species | Product design (g/kg water) | Inhibiting rate (%) | Escherichia coli detect strain number | Conclusion | |
| Contrast blank assay | Cucumber | 0 | 83 | 67 | It is exceeded |
| The present invention | Cucumber | 5 | 6 | 0 | It is qualified |
| The present invention | Cauliflower | 5 | 12 | 0 | It is qualified |
| The present invention | Rape | 5 | 9 | 0 | It is qualified |
| The present invention | Apple | 5 | 5 | 0 | It is qualified |
| The present invention | Strawberry | 5 | 10 | 0 | It is qualified |
Choose the ostreae testa pulverata obtained by embodiment 1 to dispel Bactericidal test of the residual anti-biotic material of agriculture to Escherichia coli, as a result such as
Shown in Fig. 1, it can be seen that Bactericidal test result is to have obvious inhibition zone 1,2,3,4 to produce；Represented by middle numeral 0
Be not apply the blank sample of product, do not occur inhibition zone.
Through vernier caliper measurement, antibacterial circle diameter in more than 28mm, illustrates obtained oyster shell-stealthy chlorine dioxide
Anti-biotic material is very strong to the antibacterial effect of Escherichia coli.
Claims (1)
1. the preparation method of a kind of oyster shell-stealthy chlorine dioxide anti-biotic material, it is characterised in that comprise the following steps：
The first step, first the oyster shell for banking up spontaneous fermentation purification is first cleaned up with clear water, again through drying or in gravity-flow ventilation
Under the conditions of dry in the shade, after be crushed to particle diameter be 0.5-3.5mm particle, raw material are made；
Second step, above-mentioned raw material are entered into high temperature furnace, clinker is made using three-level staged heating calcination method；Specific calcining step is such as
Under：
After being first warming up to 300-350 DEG C with 2 DEG C/min of heating rate, 10min is incubated；
Then, after being continuously heating to 650 DEG C with 5 DEG C/min of heating rate, be incubated 15-20min, then, it is aeration-cooling extremely
600℃；
After being warming up to 810-830 DEG C again with 10 DEG C/min of heating rate, 20-40min is incubated；Then, it is aeration-cooling to 750
DEG C, and 20min is incubated, produce clinker；
3rd step, clinker take out after naturally cooling to room temperature；By the clinker after cooling enter grinding machine grinding into particle diameter be 50 μm with
Under powder；
By above-mentioned by powder made from grinding and sodium chlorite powder, niter cake powder 1 ︰ 0.05-0.1 ︰ by weight
0.1-0.2 is well mixed, and is produced.
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| CN201510583056.9A CN105284882B (en) | 2015-09-15 | 2015-09-15 | A kind of oyster shell stealth chlorine dioxide anti-biotic material and preparation method thereof and application method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510583056.9A CN105284882B (en) | 2015-09-15 | 2015-09-15 | A kind of oyster shell stealth chlorine dioxide anti-biotic material and preparation method thereof and application method |
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| CN105284882A CN105284882A (en) | 2016-02-03 |
| CN105284882B true CN105284882B (en) | 2018-03-13 |
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| CN1064814C (en) * | 1995-06-29 | 2001-04-25 | 叶中良 | Bactericidal disinfectant |
| CN1244490C (en) * | 2004-09-17 | 2006-03-08 | 大连万洁日化有限公司 | Process for preparing mono package sterilizing granule capable of generating chlorine dioxide |
| CN102718247A (en) * | 2012-06-06 | 2012-10-10 | 李静 | Calcium powder and preparation method thereof |
| CN104073377A (en) * | 2014-06-12 | 2014-10-01 | 浙江海洋学院 | Method for preparing pure natural fruit and vegetable cleaning agent |
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