CN103834189A - Shark repellant and preparation method thereof - Google Patents

Shark repellant and preparation method thereof Download PDF

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Publication number
CN103834189A
CN103834189A CN201410091818.9A CN201410091818A CN103834189A CN 103834189 A CN103834189 A CN 103834189A CN 201410091818 A CN201410091818 A CN 201410091818A CN 103834189 A CN103834189 A CN 103834189A
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CN
China
Prior art keywords
shark
suction filtration
preparation
chaser
shark chaser
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN201410091818.9A
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Chinese (zh)
Inventor
许仕海
许永辉
漆天元
杨青松
严建钢
许永田
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ZHANJIANG HAIFAN SHIP NEW MATERIAL DEVELOPMENT Co Ltd
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ZHANJIANG HAIFAN SHIP NEW MATERIAL DEVELOPMENT Co Ltd
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Priority to CN201410091818.9A priority Critical patent/CN103834189A/en
Publication of CN103834189A publication Critical patent/CN103834189A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a shark repellant and a preparation method thereof, belonging to the technical field of chemical engineering. The shark repellant is prepared by adopting the steps: sulfonating oil-soluble nigrosin and fuming sulphuric acid to generate a sulfonation product; performing a dilution and neutralization process on the sulfonation product, deep phreatic water, calcium carbonate and triisobutyl carbonate, then mixing a production obtained through suction filtration, concentration and drying with cupric acetate according to a certain ratio and grinding to obtain the shark repellant. The shark repellant is powder, can be rapidly dissolved an dispersed into seawater, and releases a black-blue solution with a flavor of a copper acetate chemical, a shark can rapidly leave when in decomposed solution, thus a protection function of repelling the shark for life saving is achieved. The shark repellant is widely applicable for underwater operations, marine fishing, deep sea training and the like due to a large range of a protection region.

Description

A kind of shark chaser and preparation method thereof
Technical field
The present invention relates to a kind of shark chaser and preparation method thereof, belong to Chemicals production technical field.
Background technology
Shark, is thought one of fish the most violent in ocean by some.Approximately have in the world 380 kinds of sharks, have 30 kinds can active attack people, having 7 kinds, may to cause people injured, also has 27 kinds because the relations of build and habit have danger.Learn according to fossil investigation and scientist's reckoning, shark has lived approximately 400,000,000 years on earth, and it just existed before 400,000,000 years, and profile does not all have much changes so far, illustrates that its viability is extremely strong, person " ocean hunter ".
The most violent against great white shark in ocean, their strong lower jaw can tear up almost any prey that they are caught, and they live in the top of marine food chain.It why can attacks, is because we mankind rush in the domain of shark, just can attack us.Most of attacks occur in the waters in bank hundreds of rice off sea, and reason is very simple: most people all rests on this region after plunging into the commercial sea.
30 to 50 shark active attack events of the annual generation in the whole world, wherein have 5 to 10 causing deaths.In the U.S., Florida is that a state the most frequently occurs in attack, since nineteen ninety, all can occur every year 10 to 37.In world wide, in the number of times ranking list of shark attacks, the U.S. ranks first.Shark attack number constantly rises, and its reason is identical, is exactly that increasing people spends a holiday to seashore and participates in marine activity.Also there is no indication that shark is becoming more and more richer aggressive.
Studies show that the suitable complexity of attack motivation of shark, comprising, shark offensive attack Marine Weather situation not long ago, its feed situation, the situations such as the time length that ocean current changing conditions or even victim stop before under attack in seawater.
Shark can cause serious injury people in the time attacking.In some cases, the first of shark just can be bitten arm or leg broken completely.A surgeon is being that after a teenage Australian surfer performs an operation, the one leg that he is lost described as " just as chopper cut up with a hay cutter ".Shark exceedes 2,800 thousand grams/cm at the most advanced and sophisticated pressure producing of tooth, and large-scale shark even has than this more powerful snap-in force.
If shark does not bite people's arm or leg broken, it generally can bite a bulk of meat (tear muscle and bone) off.If shark stings on people's trunk, may make rib split, break other bone, also the skin of bulk may be torn it down.Sometimes, this can make the organ in body be exposed to outer and come to harm.
Now for the instrument that drives shark normally the external electronics of import drive shark device.Due to electronics, to drive shark device price high, maintaining difficulty, carry inconvenience, drive shark poor effect, be difficult to ensure deep ocean work personnel's life security, particularly, for the combatant through the deep-sea training of being everlasting, the shark chaser that provide reliable and secure, protection is strong becomes indispensable Protection Product.
The sense of smell of shark is very sharp, and this is to stretch to the nostril of snout both sides because there are two forks (nose capsule) brain front portion, and feeling of this fork is very sensitive.Just can rotate health and find the heavier direction of smell when It smells smell, and the source of smell is conventionally beyond 0.25 mile.
Therefore, study a kind of easy to carry, drive shark effective, there is unique lifesaving protective effect drive shark product.
Summary of the invention
The object of this invention is to provide a kind of shark chaser, this shark chaser is easy to carry, it is effective to drive shark.
Another object of the present invention is to provide a kind of preparation method of shark chaser.
In order to achieve the above object, the technical solution adopted in the present invention is:
A kind of shark chaser and preparation method thereof, comprises the steps:
(1) sulfonation
A. in dry anhydrous sulfidation pan, put into oleum, then put into 98% sulfuric acid of total inventory 2%, stir 4-6 minute, opening clamp jacket water carries out cooling;
B. add oil black nigrosine, then at 70-80 ℃ of temperature, keep stirring 0.8-1.2 hour, bleed off chuck water coolant simultaneously;
C. open chuck steam and slowly heat up, be warming up to 100-105 ℃, within insulation reaction 4-6 hour, obtain sulfonated products;
(2) dilution neutralization
A. in dilution pot, put into phreatic water, by sulfonated products progressively thread shape put into and dilute, stir simultaneously;
B. after dilution, stir 1-1.5 hour in 50-70 ℃, under stirring, slowly add the calcium carbonate of powdery to neutralize, when foam is many, carry out froth breaking with tributyl phosphate;
D. be neutralized to pH=6 ± 0.1 o'clock, blowing suction filtration, suction filtration at 50-70 ℃ of temperature;
(3) suction filtration
A. in suction filtration bucket, put suction filtration cloth bag well, then put one deck filter paper well, finally put again a filter bag, first use warm water heat once, drain, by neutralization pot and material put into suction filtration bucket and carry out suction filtration, filter pump is beaten to bin stock pot, and suction filtration for several times, obtains filtrate repeatedly;
B. use 400-500L warm water washing leaching cake, obtain washing lotion;
C. filtrate and washing lotion merging obtain amalgamation liquid, stir, and concentrate;
(4) concentrated
A. amalgamation liquid is sucked to lass lining pot and concentrate, keep pH to be less than 7;
B. be concentrated into volume 500-600L, obtain concentrated pure dye, then dry;
(5) dry
A. concentrated solution pure dye and MF auxiliary agent are mixed, enter drying room and dry;
B. bake out temperature remains on 90-100 ℃, and drying time 45-50 hour obtains finished product dyestuff after oven dry;
(6) abrasive dust blending
A. finished product drying dyestuff and venus crystals are mixed in proportion;
B. shark chaser gets product the material abrasive dust having mixed, blending after evenly;
The consumption of the oleum described in step (1) is 25-35 part, oil black nigrosine 80-120 part.
The feed time that adds oil black nigrosine described in step (1) b is 1-2 hour;
The add-on of the sulfonated products described in step (2) is 40-50 part, and the add-on of phreatic water is 15-20 part;
The add-on of the calcium carbonate described in step (2) is 30-40 part;
The described concentrated thickening temperature of step (4) is controlled at 95-100 ℃;
The concentrated solution pure dye that step (5) is described and the proportioning of MF auxiliary agent are 75:10;
The described auxiliary agent of step (5) is MF auxiliary agent;
The finished product drying dyestuff that step (6) is described and the proportioning of venus crystals are 85:15.
The invention has the beneficial effects as follows: this shark chaser protection zone scope is large, effectively protection reaches 3-4 hour, and quality validity period is 2-3.There is unique lifesaving protective effect; Can be widely used in the aspects such as underwater operation, marine fishing, deep-sea training.
Embodiment
Below by embodiment, the present invention is described in further details, these embodiment are only used for illustrating the present invention, do not limit the scope of the invention.
Embodiment 1
A kind of shark chaser and preparation method thereof, comprises the steps:
(1) sulfonation
A. in dry anhydrous sulfidation pan, put into 25 parts of oleums, then put into 98% sulfuric acid of total inventory 2%, stir 4 minutes, opening clamp jacket water carries out cooling;
B. add 80 parts of oil black nigrosines, then at 70 ℃ of temperature, keep stirring 0.8 hour, bleed off chuck water coolant simultaneously;
C. open chuck steam and slowly heat up, be warming up to 100 ℃, insulation reaction obtains sulfonated products for 4 hours;
(2) dilution neutralization
A. in dilution pot, put into 15 parts of phreatic waters, by 40 parts of sulfonated products progressively thread shape put into and dilute, stir simultaneously;
B. after dilution, stir 1 hour in 50 ℃, under stirring, slowly add 30 parts, the calcium carbonate of powdery to neutralize, when foam is many, carry out froth breaking with tributyl phosphate;
D. be neutralized to pH=6 ± 0.1 o'clock, blowing suction filtration, suction filtration at 50 ℃ of temperature;
(3) suction filtration
A. in suction filtration bucket, put suction filtration cloth bag well, then put one deck filter paper well, finally put again a filter bag, first use warm water heat once, drain, by neutralization pot and material put into suction filtration bucket and carry out suction filtration, filter pump is beaten to bin stock pot, and suction filtration for several times, obtains filtrate repeatedly;
B. use 400L warm water washing leaching cake, obtain washing lotion;
C. filtrate and washing lotion merging obtain amalgamation liquid, stir, and concentrate;
(4) concentrated
A. amalgamation liquid is sucked to lass lining pot and concentrate, keep pH to be less than 7;
B. be concentrated into volume 500L, obtain concentrated pure dye, then dry;
(5) dry
A. concentrated solution pure dye and MF auxiliary agent were mixed by 75: 10, enter drying room and dry;
B. bake out temperature remains on 90 ℃, and drying time 45 hours, obtains finished product dyestuff after oven dry;
(6) abrasive dust blending
A. finished product drying dyestuff and venus crystals are mixed in 85: 15 ratios;
B. shark chaser gets product the material abrasive dust having mixed, blending after evenly;
Embodiment 2
A kind of shark chaser and preparation method thereof, comprises the steps:
(1) sulfonation
A. in dry anhydrous sulfidation pan, put into 30 parts of oleums, then put into 98% sulfuric acid of total inventory 2%, stir 5 minutes, opening clamp jacket water carries out cooling;
B. add 100 parts of oil black nigrosines, then at 75 ℃ of temperature, keep stirring 1.0 hours, bleed off chuck water coolant simultaneously;
C. open chuck steam and slowly heat up, be warming up to 102 ℃, insulation reaction obtains sulfonated products for 5 hours;
(2) dilution neutralization
A. in dilution pot, put into 18 parts of phreatic waters, by 45 parts of sulfonated products progressively thread shape put into and dilute, stir simultaneously;
B. after dilution, stir 1.2 hours in 60 ℃, under stirring, slowly add 35 parts, the calcium carbonate of powdery to neutralize, when foam is many, carry out froth breaking with tributyl phosphate;
D. be neutralized to pH=6 ± 0.1 o'clock, blowing suction filtration, suction filtration at 60 ℃ of temperature;
(3) suction filtration
A. in suction filtration bucket, put suction filtration cloth bag well, then put one deck filter paper well, finally put again a filter bag, first use warm water heat once, drain, by neutralization pot and material put into suction filtration bucket and carry out suction filtration, filter pump is beaten to bin stock pot, and suction filtration for several times, obtains filtrate repeatedly;
B. use 450L warm water washing leaching cake, obtain washing lotion;
C. filtrate and washing lotion merging obtain amalgamation liquid, stir, and concentrate;
(4) concentrated
A. amalgamation liquid is sucked to lass lining pot and concentrate, keep pH to be less than 7;
B. be concentrated into volume 550L, obtain concentrated pure dye, then dry;
(5) dry
A. concentrated solution pure dye and MF auxiliary agent were mixed by 75: 10, enter drying room and dry;
B. bake out temperature remains on 95 ℃, and drying time 48 hours, obtains finished product dyestuff after oven dry;
(6) abrasive dust blending
A. finished product drying dyestuff and venus crystals are mixed in 85: 15 ratios;
B. shark chaser gets product the material abrasive dust having mixed, blending after evenly;
Embodiment 3
A kind of shark chaser and preparation method thereof, comprises the steps:
(1) sulfonation
A. in dry anhydrous sulfidation pan, put into 35 parts of oleums, then put into 98% sulfuric acid of total inventory 2%, stir 6 minutes, opening clamp jacket water carries out cooling;
B. add 120 parts of oil black nigrosines, then at 80 ℃ of temperature, keep stirring 1.2 hours, bleed off chuck water coolant simultaneously;
C. open chuck steam and slowly heat up, be warming up to 105 ℃, insulation reaction obtains sulfonated products for 6 hours;
(2) dilution neutralization
A. in dilution pot, put into 20 parts of phreatic waters, by 50 parts of sulfonated products progressively thread shape put into and dilute, stir simultaneously;
B. after dilution, stir 1.5 hours in 70 ℃, under stirring, slowly add 40 parts, the calcium carbonate of powdery to neutralize, when foam is many, carry out froth breaking with tributyl phosphate;
D. be neutralized to pH=6 ± 0.1 o'clock, blowing suction filtration, suction filtration at 70 ℃ of temperature;
(3) suction filtration
A. in suction filtration bucket, put suction filtration cloth bag well, then put one deck filter paper well, finally put again a filter bag, first use warm water heat once, drain, by neutralization pot and material put into suction filtration bucket and carry out suction filtration, filter pump is beaten to bin stock pot, and suction filtration for several times, obtains filtrate repeatedly;
B. use 500L warm water washing leaching cake, obtain washing lotion;
C. filtrate and washing lotion merging obtain amalgamation liquid, stir, and concentrate;
(4) concentrated
A. amalgamation liquid is sucked to lass lining pot and concentrate, keep pH to be less than 7;
B. be concentrated into volume 600L, obtain concentrated pure dye, then dry;
(5) dry
A. concentrated solution pure dye and MF auxiliary agent were mixed by 75: 10, enter drying room and dry;
B. bake out temperature remains on 100 ℃, and drying time 50 hours, obtains finished product dyestuff after oven dry;
(6) abrasive dust blending
A. finished product drying dyestuff and venus crystals are mixed in 85: 15 ratios;
B. shark chaser gets product the material abrasive dust having mixed, blending after evenly;
Embodiment 4
The technical indicator of shark chaser and detection method
Shark chaser technical indicator (being standard-required)
Index name Technical requirements
Outward appearance The even powder of black or reddish black
Intensity ≥100%
Solubleness ≤180S ec
Diffustivity ≤120S ec
Moisture content ≤10%
Fineness More than 95% pass through 100 ~ 120 orders
PH 5~6
Coloured light Micro-orchid
1. the mensuration of intensity (visual colorimetry)
With weighing bottle sample thief 0.5000g, be dissolved in natural sea-water, in rear immigration 500ml volumetric flask to be dissolved, and thousand hammer hundred be diluted to scale, get the former shark chaser 6616 of solution 10ml(and get 7.5ml) in 100ml volumetric flask, be diluted to scale with natural sea-water, after shaking up, contain the colorimetric cylinder into 100ml, contrast with concentration known.Sample liquid with range estimation relatively, is evaluated its concentration conversion to being equal to standard model percentum (>=100%th, qualified product).
Calculation formula:
Sample intensity (being concentration %)-100 × 10/x
100 standard model concentration x are ml numbers of the ml number 10 standard model solution of detected solution.
2. the mensuration of solubleness (Nacl solution is determined method)
On analytical balance, take 6616 of the former shark chasers of sample 10mg(and need 7.5mg) in beaker, pour natural sea-water (8%Nacl solution) 100ml into, after slightly stirring, pour in colorimetric cylinder and observe, be clear solution and color depth if 180Sec can dissolve completely, solubleness is good, is qualified product; Do not dissolve fine powder if having on a small quantity, look darker, solubleness is better, does not morely dissolve fine powder, look shallow, poor solubility if having.
3. diffusion (observation)
In 400ml beaker, contain 400ml natural sea-water, with stainless steel key sampling 2mg(synthetics+agent mixture+CuAc), flip rim of a cup and fall apart to the water surface, slightly gently stir the water surface, observe its diffusion sinking situation, if sink to being full of beaker at 160See internal diffusion, to there is no granule foreign be qualified product.
4. the mensuration of moisture content (roasting dry method)
Accurately take sample 10g and put into a dry glass device, be placed in baking box at 50 ~ 55 ℃, bake to constant weight (general 12 hours), take out and put into moisture eliminator cooling 15 minutes, then weigh, calculate its moisture content, if water content≤10%, qualified product.Moisture content (%)=[(sample roasting dry front heavy-sample is roasting dry rear heavy)/sample is roasting dry front heavy] × 100%.
5.PH pH-value determination pH PHS-25 type PH counts assay method)
Accurately take 10ng sample, put in the beaker that fills 100ml distilled water and mix rear insertion PH meter probe, if detected result is qualified product within the scope of pH value 5-6.

Claims (10)

1. a preparation method for shark chaser, is characterized in that: comprise the steps:
(1) sulfonation
A. in dry anhydrous sulfidation pan, put into oleum, then put into 98% sulfuric acid of total inventory 2%, stir 4-6 minute, opening clamp jacket water carries out cooling;
B. add oil black nigrosine, then at 70-80 ℃ of temperature, keep stirring 0.8-1.2 hour, bleed off chuck water coolant simultaneously;
C. open chuck steam and slowly heat up, be warming up to 100-105 ℃, within insulation reaction 4-6 hour, obtain sulfonated products;
(2) dilution neutralization
A. in dilution pot, put into phreatic water, by sulfonated products progressively thread shape put into and dilute, stir simultaneously;
B. after dilution, stir 1-1.5 hour in 50-70 ℃, under stirring, slowly add the calcium carbonate of powdery to neutralize, when foam is many, carry out froth breaking with tributyl phosphate;
D. be neutralized to pH=6 ± 0.1 o'clock, blowing suction filtration, suction filtration at 50-70 ℃ of temperature;
(3) suction filtration
A. in suction filtration bucket, put suction filtration cloth bag well, then put one deck filter paper well, finally put again a filter bag, first use warm water heat once, drain, by neutralization pot and material put into suction filtration bucket and carry out suction filtration, filter pump is beaten to bin stock pot, and suction filtration for several times, obtains filtrate repeatedly;
B. use 400-500L warm water washing leaching cake, obtain washing lotion;
C. filtrate and washing lotion merging obtain amalgamation liquid, stir, and concentrate;
(4) concentrated
A. amalgamation liquid is sucked to lass lining pot and concentrate, keep pH to be less than 7;
B. be concentrated into volume 500-600L, obtain concentrated pure dye, then dry;
(5) dry
A. concentrated solution pure dye and MF auxiliary agent are mixed, enter drying room and dry;
B. bake out temperature remains on 90-100 ℃, and drying time 45-50 hour obtains finished product dyestuff after oven dry;
(6) abrasive dust blending
A. finished product drying dyestuff and venus crystals are mixed in proportion;
B. shark chaser gets product the material abrasive dust having mixed, blending after evenly.
2. the preparation method of a kind of shark chaser according to claim 1, is characterized in that: the consumption of the oleum described in step (1) is 25-35 part, oil black nigrosine 80-120 part.
3. the preparation method of a kind of shark chaser according to claim 1, is characterized in that: the feed time that adds oil black nigrosine described in step (1) b is 1-2 hour.
4. the preparation method of a kind of shark chaser according to claim 1, is characterized in that: the add-on of the sulfonated products described in step (2) is 40-50 part, and the add-on of phreatic water is 15-20 part.
5. the preparation method of a kind of shark chaser according to claim 1, is characterized in that: the add-on of the calcium carbonate described in step (2) is 30-40 part.
6. the preparation method of a kind of shark chaser according to claim 1, is characterized in that: the described concentrated thickening temperature of step (4) is controlled at 95-100 ℃.
7. the preparation method of a kind of shark chaser according to claim 1, is characterized in that: the concentrated solution pure dye that step (5) is described and the proportioning of MF auxiliary agent are 75:10.
8. according to the preparation method of a kind of shark chaser described in claim 1 or 7, it is characterized in that: the described auxiliary agent of step (5) is MF auxiliary agent.
9. the preparation method of a kind of shark chaser according to claim 1, is characterized in that: the finished product drying dyestuff that step (6) is described: venus crystals=85:15.
10. a shark chaser, is characterized in that: the shark chaser that described in this shark chaser employing claim 1 prepared by method.
CN201410091818.9A 2014-03-13 2014-03-13 Shark repellant and preparation method thereof Pending CN103834189A (en)

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CN103834189A true CN103834189A (en) 2014-06-04

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106879612A (en) * 2017-03-07 2017-06-23 湛江市海帆船舶新材料开发有限公司 A kind of shark chaser and preparation method thereof

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US20060024344A1 (en) * 2004-07-12 2006-02-02 Matos Gonzalo R Capsicum shark repellent
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CN101817791A (en) * 2009-02-27 2010-09-01 严纪一 Method for directly producing water soluble aniline black

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JP2907817B1 (en) * 1998-06-17 1999-06-21 ヤマヤ産業株式会社 Underwater animal threat system
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WO2006135876A2 (en) * 2005-06-11 2006-12-21 Shark Defense Llc Elasmobranch-repelling compounds and methods of use
US20090061012A1 (en) * 2007-06-24 2009-03-05 Anthony Neville Drew Shark Repelling Method and Repellent Incorporating Wax
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CN101817791A (en) * 2009-02-27 2010-09-01 严纪一 Method for directly producing water soluble aniline black

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CN106879612A (en) * 2017-03-07 2017-06-23 湛江市海帆船舶新材料开发有限公司 A kind of shark chaser and preparation method thereof

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Application publication date: 20140604