CN106721624A - A kind of anti-oxidant heavy property aquatic products food calling particle and preparation method thereof - Google Patents
A kind of anti-oxidant heavy property aquatic products food calling particle and preparation method thereof Download PDFInfo
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- CN106721624A CN106721624A CN201611112508.6A CN201611112508A CN106721624A CN 106721624 A CN106721624 A CN 106721624A CN 201611112508 A CN201611112508 A CN 201611112508A CN 106721624 A CN106721624 A CN 106721624A
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Abstract
The present invention relates to aquaculture field, a kind of anti-oxidant heavy property aquatic products food calling particle and preparation method thereof is disclosed, the aquatic products food calling particle contains phagostimulant and anti-oxidant modified shell particles；The preparation method of anti-oxidant modified shell particles is as follows：Aluminium block, MAG block, spelter are weighed, and is put into dissolving in excessive dilute nitric acid solution, again to silver nitrate is added in solution after being completely dissolved, then adjust pH to neutrality, obtain multiple metal ion solution；Multiple metal ion solution is stirred at 85 95 DEG C, to shell particles are added in solution, 100 110 DEG C, after the 2h of standing adsorption 1 is warming up to, shell particles are taken out, drying obtains anti-oxidant modified shell particles.Food calling particle of the invention contains antioxidant content, is prevented from phagostimulant and oxidation and breed bacteria occur, and long shelf-life, the phagostimulating effect after dispensing is also more preferable.
Description
Technical field
The present invention relates to aquaculture field, more particularly to a kind of anti-oxidant heavy property aquatic products food calling particle and its preparation side
Method.
Background technology
At present, the aquatic feeds of culture fishery mainly have two kinds of sinking feed and buoyancy feed.Buoyancy feed is then
The water surface can be floated up to foster rear feed granules are thrown, aquatic biological is ingested at approximately level, and user can well observe aquatic products
Situation of ingesting, effectively control feed throwing support amount.But because feed floats up to the water surface after throwing is supported, aquatic biological is necessary
Ingested in superjacent waters, and for centering, lower floor's aquatic biological, be then unfavorable for that it is ingested and increased physical consumption.Heavy property is raised
The particle of material can be settled after feeding, the aquatic biological for living in middle lower floor is smoothly ingested.
Phagostimulant is the adjuvant for mixed feed, it is possible to increase hobby of the aquiculture animal to feed, is improved
It takes the photograph bait rate, reduces feed waste, improves feed efficiency.Although the aquatic feeds nutrition that current industrial metaplasia is produced is very comprehensively,
By not being food that aquiculture animal was had a liking for originally, many feeds are not eaten and are wasted.Therefore typically will can all lure
Food agent is delivered with feed formulation or directly phagostimulant is added in feed.The principle of phagostimulant is：Most aquiculture animals
Vision it is undeveloped, they rely primarily on smell life.Phagostimulant is added in feed, phagostimulant can lure that aquaculture is moved into
Thing is concentrated on around feed, and then causes the appetite of aquiculture animal, and promotes it to complete feed of eating.
The main component of current phagostimulant is general amino acid, nucleotides, glycine betaine, organic acid, SCFA etc.,
These materials are susceptible to oxidation and easily breed bacteria after storage or dispensing, thus go bad, it is corrupt, lead
Cause the reduction of phagostimulant phagostimulating effect even entirely ineffective.Chinese patent such as Application No. 200910154219.6 discloses one kind
Artificial bait for tunny and its special slow release phagostimulant.Wherein, the slow release phagostimulant is solidifying containing 1 to 10 part of sustained release by weight
Glue, 0.5 to 1 part of food calling bait, 1 to 50 part of water.What sustained-release gel played a part of is the dissolving for slowing down food calling bait, according to
Actual conditions can indirectly adjust the speed of sustained release by adjusting the ratio of water.Therefore, the invention with smell lure the time it is long,
Cheap, pollution less, the good advantage of trap effect.
The food calling bait of the phagostimulant is susceptible to oxidation and breed bacteria, and not only the shelf-life is short, and after dispensing
Phagostimulating effect is also affected.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides the anti-oxidant heavy property aquatic products food calling particle of one kind and its preparation side
Method.Food calling particle of the invention contains antioxidant content, is prevented from phagostimulant and oxidation and breed bacteria, shelf-life occur
Long, the phagostimulating effect after dispensing is also more preferable.
Additionally, food calling grain density of the present invention is larger, with heavy property, the sink-float with heavy property aquatic feeds is consistent；
And the food calling particle can realize multistage controlled release so that phagostimulant rate of release is more homogeneous, stabilization, phagostimulating effect is good, lures
Food timeliness is long.
Concrete technical scheme of the invention is：
A kind of anti-oxidant heavy property aquatic products food calling particle, changes containing phagostimulant and as the anti-oxidant of food calling agent carrier
Property shell particles.
The preparation method of the anti-oxidant modified shell particles is as follows：Aluminium block, MAG block, spelter are weighed, and is put into
Dissolved in excessive dilute nitric acid solution, again to silver nitrate is added in solution after being completely dissolved, then adjust pH to neutrality, obtain many
First metal ion solution；Multiple metal ion solution is stirred at 85-95 DEG C, to shell particles are added in solution, is risen
Temperature after standing adsorption 1-2h, takes out shell particles to 100-110 DEG C, and drying obtains anti-oxidant modified shell particles.
The present invention carries out anti-oxidant modified to shell particles.In modifying process, by aluminium block, MAG block, spelter dust technology
Dissolving, generates multiple metal ion solution and hydrogen.Although most hydrogen directly can escape from solution, solution
In or a small amount of hydrogen can be contained.Addition silver nitrate after, addition shell particles the multiple metal ion in solution is carried out from
Son exchange, adsorbing metal ions and hydrogen.Anti-oxidant modified shell particles are finally obtained.Wherein, hydrogen has stronger reduction
Property, can not only strengthen the oxidation resistance of food calling particle, extend the shelf life, even and if after aquatic livestock eats, it is also nontoxic
Evil, can also improve the oxidation resistance of aquatic livestock cell, so as to improve its immunocompetence on the contrary.Additionally, anti-oxidant modified shellfish
Due to containing multiple metal ion, with stronger antibacterial ability, its principle is shell particle：Presence and difference due to hydrogen
Potential difference between metal ion, can form galvanic effect in water after dispensing, generate a large amount of negative hydrogen ions, improve antibacterial
Activity.And, these polybasic ions can also be supplemented after being eaten by aquiculture animal as trace element, be built up health.
Further, the mol ratio of aluminium ion, magnesium ion, zinc ion and silver ion is in the multiple metal ion solution
0.5-1.5:0.5-1.5:0.5-1.5:0.5-1.5。
Further, the mass concentration of the dust technology is 20-40%.
Further, the quality of the shell particles is 0.5-1.5 times of multiple metal ion solution.
Further, the preparation method of the shell particles is：Shell is cleaned, is transferred in Muffle furnace, in 300-400
1-2h is calcined at DEG C；Cooling is taken out after roasting, shell is ground into the shell particles of 40-80 mesh.
In the present invention, shell is first calcined, it is necessary to considered critical sintering temperature and time in roasting process,
The purpose being calcined in the present invention clearly, is calcined 1-2h at 300-400 DEG C, and the organic matter in shell is decomposed, and it is occupied
Space be released, shell is internally formed the pore passage structure of a large amount of micron levels, above-mentioned being formed after being calcined under technique
Duct, dimensional homogeneity is good, with outstanding adsorptivity, and is mutual between its duct compared with the routine carrier such as activated carbon
Connection, be usually duct single, disconnected with each other rather than such as activated carbon, therefore its adsorbance is bigger, slow release effect
More preferably.
Further, the shell particles are also by activation process：It is the citric acid solution of 6-6.5 to prepare pH, by shell
Particle soaks 3-5h in the citric acid solution of its 8-12 times of quality, and soaking temperature is 40-50 DEG C；Taken out after immersion, dried, obtained
To the shell particles of activation process.
The absorption property of shell particles is more preferably after activation process.
Further, the aquatic products food calling particle is in hud typed, core part include the raw material of following weight portion be blended and
Into：Phagostimulant 45-55 parts, anti-oxidant modified shell particles 20-24 parts, Hydroxypropyl methylcellulose 17-21 parts, prominent release agent 3-5 part, glue
Mixture 2-4 parts, lubricant 1-3 parts；Shell sections include that the raw material of following weight portion is blended：Phagostimulant 45-55 parts, antioxygen
Change modified 17-21 parts of shell particles, Hydroxypropyl methylcellulose 8-12 parts, retarding agent 14-18 parts, adhesive 2-4 parts, lubricant 1-3
Part；The core part is 1 with the mass ratio of shell sections:4-10.
Existing phagostimulant, typically all directly adds directly as feed addictive in feed granulation process, though
So so it is able to ensure that the uniformity with feed sink-float property.But it does not possess slow releasing function.And some be carried on density compared with
On small carrier, although with certain slow release effect, but its density is smaller, will be floated rapidly in an input water body.
Food calling particle of the invention, is main sustained-release matrix with shell particles and Hydroxypropyl methylcellulose, wherein anti-oxidant modified shell
Intragranular portion has substantial amounts of pore passage structure, and with preferable adsorptivity, the load capacity to phagostimulant is big, with preferable controlled release effect
Really.And anti-oxidant modified shell particles easily adsorb water, being flooded food calling particle after moistening will rest on the middle bottom of water.
On the other hand, existing phagostimulant, its controlled capability is poor：Some phagostimulants, easily cause after delivering in water
Initial stage meets water and largely dissolves, and causes to dash forward and releases situation, causes food calling timeliness short.Although some phagostimulant food calling timeliness are more long,
Its rate of release is excessively slow, it is impossible to fully play a part of food calling.On the other hand, existing phagostimulant, the phase is due to luring upon discharge
The surface area that the reduction of food calling component content and phagostimulant are contacted with water in food agent reduces, and can there is the release of later stage food calling composition
Situation about being short of power, food calling constituent concentration is too low in causing its region water, it is impossible to play enough phagostimulating effects.
Food calling particle of the invention is hud typed, and shell sections are different from the rate of release of core part：Shell sections
Phagostimulant rate of release rationally, will not early period of origination be prominent releases situation.Core part can speed up the release to phagostimulant, after overcoming
The defect that the release of phase phagostimulant is short of power, improves phagostimulating effect.
Concrete principle of the invention is：
The primary raw material of shell sections has：Phagostimulant, anti-oxidant modified shell particles, Hydroxypropyl methylcellulose, retarding agent.Its
In, anti-oxidant modified shell particles and Hydroxypropyl methylcellulose are respectively as the carrier of phagostimulant, and the drugloading rate to phagostimulant is high, and
All there is slow-release function.Water-soluble due to Hydroxypropyl methylcellulose can dissolve rapidly relatively by force after meeting water, easily cause early stage and dash forward
Release, therefore add retarding agent, limit the quick dissolving of Hydroxypropyl methylcellulose, reduce the early stage rate of release of phagostimulant.
Core part includes：Phagostimulant, anti-oxidant modified shell particles, Hydroxypropyl methylcellulose, prominent release agent.With shell portion
Point gradually dissolving, be gradually exposed in anaphase nucleus core segment, prominent in core part releases agent has the effect of moisture absorption heat release
Really, dash forward after releasing agent moisture absorption heat release, cause Hydroxypropyl methylcellulose to accelerate dissolving, so that accelerate the release of phagostimulant, after overcoming controlled release
The defect that the release of phase phagostimulant is short of power.
Further, the phagostimulant is selected from the one kind in amino acid, nucleotides, glycine betaine, organic acid, SCFA
Or it is various；The retarding agent is ethyl cellulose, and ethyl cellulose solubility in water is smaller, can slow down Hydroxypropyl methylcellulose
Dissolving.Described adhesive is selected from one or more in polyvinylpyrrolidone, sodium carboxymethylcellulose；The lubricant choosing
One or more from talcum powder, magnesium stearate, superfine silica gel powder.
Further, the viscosity of the Hydroxypropyl methylcellulose is 6000-10000mps.
The slow release effect of the Hydroxypropyl methylcellulose of the range of viscosities and the processing in preparation process are ideal.
Further, it is described it is prominent release agent preparation method be：
By quick lime powder and ethylene glycol in mass ratio 10:2-3 is mixed and stirred for uniformly, then adds at 130-140 DEG C
Pressure heating stirring reaction 2-3h；The butyl lithium of quick lime powder quality 3-4% is added during 0.5-1h is reacted, reaction terminates
After product is cooled to room temperature, be obtained and prominent release agent.
Dashed forward obtained in the above method and release agent, be under the catalysis of butyl lithium, to gather in the surface aggregate generation of quick lime powder
Oxirane layer, quick lime has good hygroscopicity, and calcium hydroxide is generated after chance water and heat is discharged, and these heats can add
The dissolving of fast Hydroxypropyl methylcellulose, accelerates the release of phagostimulant.But if quick lime is more violent with a large amount of water direct reactions, meeting
Cause temperature too high, be this in quick lime Surface Creation PEO layer, PEO layer plays iris action, prominent to release agent
Water needs to be reacted with quick lime after penetrating into PEO layer after meeting water, greatly reduces reaction acutely degree.
And because PEO layer is to the parcel of quick lime powder, even if quick lime is violent with water reaction, also play obstruct and
The effect of buffering.
Further, the Hydroxypropyl methylcellulose in the shell sections is by modification：
Hydroxypropyl methylcellulose is mixed with anhydrous dimethylacetamide by solid-to-liquid ratio 1g/30mL-1g/15mL, 55- is heated to
65 DEG C dissolve Hydroxypropyl methylcellulose, then in solution add quality for 1-1.5 times of Hydroxypropyl methylcellulose stearyl chloride with
Quality is the triethylamine of 0.2-0.3 times of Hydroxypropyl methylcellulose, and stirring is vacuumized under inert gas shielding；Then solution is shifted
Into 30-35 DEG C of water-bath 4-10h is reacted under inert gas shielding；Product is added in enough absolute ethyl alcohols after reaction
Precipitated, filtration under diminished pressure after precipitation, take solid and preliminary modified hypromellose is successively obtained after cleaning, drying
Element；Preliminary modified Hydroxypropyl methylcellulose is added in the glyoxal water solution that mass concentration is 6-8%, wherein preliminary modified
10-20 times of quality and ethylene glycol of Hydroxypropyl methylcellulose, the stirring reaction 1-3h at a temperature of 30-40 DEG C is eventually passed and washed
Wash, dry after obtain twice-modified Hydroxypropyl methylcellulose.
To Hydroxypropyl methylcellulose by after further modification, can further improve its slow release effect, change for the first time
Property after, the end group of Hydroxypropyl methylcellulose contains part hydrophobic grouping, its water solubility reduce；After twice-modified, hypromellose
Element there occurs a certain degree of precrosslink, therefore it is not easy to meet water at the dispensing initial stage and dissolves rapidly, at the same also improve its
Stability under different pH environment.In addition above-mentioned method of modifying low toxicity is harmless, meets the use requirement of feed addictive.
The preparation method of above-mentioned anti-oxidant heavy property aquatic products food calling particle, comprises the following steps：
1) preparation of core part：Each raw material is weighed by proportioning, each component is sieved respectively；By anti-oxidant modified shell
Grain is added water and stirs, and is made the suspension that concentration is 5-15wt%, and the phagostimulant of 1/2-1/3 amounts is added under agitation,
Absorption 6-8h, after centrifugation, drying, obtains being adsorbed with the anti-oxidant modified shell particles of phagostimulant；By remaining phagostimulant, absorption
Have the anti-oxidant modified shell particles of phagostimulant, Hydroxypropyl methylcellulose, it is prominent release agent and be well mixed, adhesive ethanol is dissolved；
Granulated after above-mentioned well mixed raw material is mixed with adhesive, after drying, sieve grain, add mix lubricant uniform.
2) preparation of shell：Each raw material is weighed by proportioning, each component is sieved respectively；Anti-oxidant modified shell particles are added
Water is stirred, and is made the suspension that concentration is 5-15wt%, and the phagostimulant of 1/2-1/3 amounts, absorption are added under agitation
6-8h, after centrifugation, drying, obtains being adsorbed with the anti-oxidant modified shell particles of phagostimulant；By remaining phagostimulant, it is adsorbed with and lures
The anti-oxidant modified shell particles of food agent, Hydroxypropyl methylcellulose, retarding agent are well mixed, and adhesive ethanol is dissolved；Will be upper
State well mixed raw material and step 1) obtained by core part, adhesive granulated after being well mixed, drying, sieve grain
Afterwards, add mix lubricant uniform, finished product.
Further, the phagostimulant crosses 200 mesh sieves, and the anti-oxidant modified shell particles cross 40-80 mesh sieves, the hydroxyl
Third methylcellulose, prominent release agent, retarding agent and cross 80 mesh sieves.The lubricant crosses 80 mesh sieves.
The beneficial effects of the invention are as follows：Food calling particle of the invention contains antioxidant content, is prevented from phagostimulant generation
Oxidation and breed bacteria, long shelf-life, the phagostimulating effect after dispensing are also more preferable.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of anti-oxidant heavy property aquatic products food calling particle, in hud typed.
Core part includes that the raw material of following weight portion is blended：It is 50 parts of phagostimulant (amino acid, nucleotides), anti-oxidant
Modified 22 parts of shell particles, 19 parts of Hydroxypropyl methylcellulose (viscosity is 6000-10000mps), prominent release 4 parts of agent, adhesive (poly- second
Alkene pyrrolidone) 3 parts, 2 parts of lubricant (talcum powder).
Shell sections include that the raw material of following weight portion is blended：It is 50 parts of phagostimulant (amino acid, nucleotides), anti-oxidant
Modified 19 parts of shell particles, 10 parts of Hydroxypropyl methylcellulose (viscosity is 6000-10000mps), retarding agent (ethyl cellulose) 16
Part, 3 parts of adhesive (polyvinylpyrrolidone), 2 parts of lubricant (talcum powder)；The core part and the mass ratio of shell sections
It is 1:7.
In the present embodiment,
The preparation method of the anti-oxidant modified shell particles is：
Shell is cleaned, is transferred in Muffle furnace, 1.5h is calcined at 350 DEG C；Cooling is taken out after roasting, shell is crushed
Into the shell particles of 40-80 mesh.It is the citric acid solution of 6-6.5 separately to prepare pH, by shell particles in its 10 times of lemons of quality
4h is soaked in lemon acid solution, soaking temperature is 45 DEG C；Taken out after immersion, dried, obtain the shell particles of activation process.
Weigh aluminium block, MAG block, spelter, and put into molten in the dilute nitric acid solution that excessive mass concentration is 30%
Solution, again to silver nitrate is added in solution after being completely dissolved, then adjusts pH to neutrality, obtains multiple metal ion solution, solution
The mol ratio of middle aluminium ion, magnesium ion, zinc ion and silver ion is 1:1:1:1；Multiple metal ion solution is stirred at 90 DEG C
Mix uniform, to the shell particles that 1 times of solution quality is added in solution, be warming up to 105 DEG C, after standing adsorption 1.5h, take out shell
Particle, drying obtains anti-oxidant modified shell particles.
It is described it is prominent release agent preparation method be：
By quick lime powder and ethylene glycol in mass ratio 10:2.5 are mixed and stirred for uniformly, and then pressurization adds at 135 DEG C
2.5h is reacted in thermal agitation；The butyl lithium of quick lime powder quality 3.5% is added during 0.75h is reacted, reaction makes after terminating
Product is cooled to room temperature, is obtained to dash forward and releases agent.
A kind of preparation method of anti-oxidant heavy property aquatic products food calling particle, comprises the following steps：
1) preparation of core part：Each raw material is weighed by proportioning, each component is sieved respectively, and (phagostimulant crosses 200 mesh sieves, resists
Oxidation modification shell particles cross 40-80 mesh sieves, Hydroxypropyl methylcellulose, prominent release agent, retarding agent and cross 80 mesh sieves.Lubricant crosses 80 mesh
Sieve)；Anti-oxidant modified shell particles are added water and is stirred, be made the suspension that concentration is 10wt%, added under agitation
Enter the phagostimulant of 1/2 amount, adsorb 7h, after centrifugation, drying, obtain being adsorbed with the anti-oxidant modified shell particles of phagostimulant；Will be surplus
Remaining phagostimulant, the anti-oxidant modified shell particles for being adsorbed with phagostimulant, Hydroxypropyl methylcellulose, it is prominent release agent and be well mixed, will be viscous
Mixture ethanol dissolves；Granulated after above-mentioned well mixed raw material is mixed with adhesive, after drying, sieve grain, added
Mix lubricant is uniform.
2) preparation of shell：Each raw material is weighed by proportioning, each component is sieved respectively, and (phagostimulant crosses 200 mesh sieves, anti-oxidant
Modified shell particles cross 40-80 mesh sieves, Hydroxypropyl methylcellulose, prominent release agent, retarding agent and cross 80 mesh sieves.Lubricant crosses 80 mesh sieves)；Will
Anti-oxidant modified shell particles are added water and stir, and are made the suspension that concentration is 10wt%, and 1/2 amount is added under agitation
Phagostimulant, adsorb 7h, centrifugation, dry after, obtain being adsorbed with the anti-oxidant modified shell particles of phagostimulant；By remaining food calling
Agent, the anti-oxidant modified shell particles for being adsorbed with phagostimulant, Hydroxypropyl methylcellulose, retarding agent are well mixed, by adhesive second
Alcohol dissolves；By above-mentioned well mixed raw material and step 1) obtained by core part, adhesive granulated after being well mixed, then pass through
After dry, sieve grain, add mix lubricant uniform, finished product.
Embodiment 2
A kind of anti-oxidant heavy property aquatic products food calling particle, in hud typed.
Core part includes that the raw material of following weight portion is blended：Phagostimulant (glycine betaine, organic acid, SCFA)
45 parts, 24 parts of anti-oxidant modified shell particles, 21 parts of Hydroxypropyl methylcellulose (viscosity is 6000-10000mps), it is prominent release 5 parts of agent,
4 parts of adhesive (sodium carboxymethylcellulose), 1 part of lubricant (magnesium stearate).
Shell sections include that the raw material of following weight portion is blended：Phagostimulant (glycine betaine, organic acid, SCFA)
45 parts, 21 parts of anti-oxidant modified shell particles, 12 parts of Hydroxypropyl methylcellulose (viscosity is 6000-10000mps), retarding agent (ethyl
Cellulose) 18 parts, 2 parts of adhesive (sodium carboxymethylcellulose), 2 parts of lubricant (magnesium stearate)；The core part and shell
Partial mass ratio is 1:10.
In the present embodiment,
The preparation method of the anti-oxidant modified shell particles is：
Shell is cleaned, is transferred in Muffle furnace, 2h is calcined at 300 DEG C；Cooling is taken out after roasting, shell is ground into
The shell particles of 40-80 mesh.
Weigh aluminium block, MAG block, spelter, and put into molten in the dilute nitric acid solution that excessive mass concentration is 20%
Solution, again to silver nitrate is added in solution after being completely dissolved, then adjusts pH to neutrality, obtains multiple metal ion solution, solution
The mol ratio of middle aluminium ion, magnesium ion, zinc ion and silver ion is 0.5:.5:0.5:1.5；By multiple metal ion solution 85
Stirred at DEG C, to the shell particles that 0.5 times of solution quality is added in solution, be warming up to 100 DEG C, after standing adsorption 1h, taken
Go out shell particles, drying obtains anti-oxidant modified shell particles.
It is described it is prominent release agent preparation method be：
By quick lime powder and ethylene glycol in mass ratio 10:2 are mixed and stirred for uniformly, then the pressurized, heated at 130 DEG C
Stirring reaction 3h；The butyl lithium of quick lime powder quality 3% is added during 0.5h is reacted, reaction makes product after terminating
Room temperature is cooled to, is obtained to dash forward and is released agent.
A kind of preparation method of anti-oxidant heavy property aquatic products food calling particle, comprises the following steps：
1) preparation of core part：Each raw material is weighed by proportioning, each component is sieved respectively, and (phagostimulant crosses 200 mesh sieves, resists
Oxidation modification shell particles cross 40-80 mesh sieves, Hydroxypropyl methylcellulose, prominent release agent, retarding agent and cross 80 mesh sieves.Lubricant crosses 80 mesh
Sieve)；Anti-oxidant modified shell particles are added water and is stirred, be made the suspension that concentration is 5wt%, added under agitation
The phagostimulant of 1/3 amount, adsorbs 6h, after centrifugation, drying, obtains being adsorbed with the anti-oxidant modified shell particles of phagostimulant；By residue
Phagostimulant, be adsorbed with phagostimulant anti-oxidant modified shell particles, Hydroxypropyl methylcellulose, it is prominent release agent and be well mixed, will bond
Agent ethanol dissolves；Granulated after above-mentioned well mixed raw material is mixed with adhesive, after drying, sieve grain, add profit
Lubrication prescription is well mixed.
2) preparation of shell：Each raw material is weighed by proportioning, each component is sieved respectively, and (phagostimulant crosses 200 mesh sieves, anti-oxidant
Modified shell particles cross 40-80 mesh sieves, Hydroxypropyl methylcellulose, prominent release agent, retarding agent and cross 80 mesh sieves.Lubricant crosses 80 mesh sieves)；Will
Anti-oxidant modified shell particles are added water and stir, and are made the suspension that concentration is 5wt%, and 1/3 amount is added under agitation
Phagostimulant, adsorb 6h, centrifugation, dry after, obtain being adsorbed with the anti-oxidant modified shell particles of phagostimulant；By remaining food calling
Agent, the anti-oxidant modified shell particles for being adsorbed with phagostimulant, Hydroxypropyl methylcellulose, retarding agent are well mixed, by adhesive second
Alcohol dissolves；By above-mentioned well mixed raw material and step 1) obtained by core part, adhesive granulated after being well mixed, then pass through
After dry, sieve grain, add mix lubricant uniform, finished product.
Embodiment 3
A kind of anti-oxidant heavy property aquatic products food calling particle, in hud typed.
Core part includes that the raw material of following weight portion is blended：It is 50 parts of phagostimulant (amino acid, nucleotides), anti-oxidant
Modified 22 parts of shell particles, 19 parts of Hydroxypropyl methylcellulose (viscosity is 6000-10000mps), prominent release 4 parts of agent, adhesive (poly- second
Alkene pyrrolidone, sodium carboxymethylcellulose) 3 parts, 2 parts of lubricant (superfine silica gel powder).
Shell sections include that the raw material of following weight portion is blended：50 parts of phagostimulant (SCFA), anti-oxidant change
19 parts of shell particles of property, 10 parts of Hydroxypropyl methylcellulose (viscosity is 6000-10000mps), 16 parts of retarding agent (ethyl cellulose),
3 parts of adhesive (polyvinylpyrrolidone, sodium carboxymethylcellulose), 2 parts of lubricant (superfine silica gel powder)；The core part and shell
The mass ratio of layer segment is 1:7.
In the present embodiment,
The preparation method of the anti-oxidant modified shell particles is：
Shell is cleaned, is transferred in Muffle furnace, 1.5h is calcined at 350 DEG C；Cooling is taken out after roasting, shell is crushed
Into the shell particles of 40-80 mesh.It is the citric acid solution of 6-6.5 separately to prepare pH, by shell particles in its 10 times of lemons of quality
4h is soaked in lemon acid solution, soaking temperature is 45 DEG C；Taken out after immersion, dried, obtain the shell particles of activation process.
Weigh aluminium block, MAG block, spelter, and put into molten in the dilute nitric acid solution that excessive mass concentration is 40%
Solution, again to silver nitrate is added in solution after being completely dissolved, then adjusts pH to neutrality, obtains multiple metal ion solution, solution
The mol ratio of middle aluminium ion, magnesium ion, zinc ion and silver ion is 1.5:0.5:1.5:0.5；Multiple metal ion solution is existed
Stirred at 95 DEG C, to the shell particles that 1.5 times of solution quality is added in solution, be warming up to 110 DEG C, after standing adsorption 2h,
Shell particles are taken out, drying obtains anti-oxidant modified shell particles.
It is described it is prominent release agent preparation method be：
By quick lime powder and ethylene glycol in mass ratio 10:3 are mixed and stirred for uniformly, then the pressurized, heated at 140 DEG C
Stirring reaction 2h；The butyl lithium of quick lime powder quality 4% is added during 1h is reacted, reaction makes product cold after terminating
But to room temperature, it is obtained to dash forward and releases agent.
The Hydroxypropyl methylcellulose in the shell sections is by modification：
Hydroxypropyl methylcellulose is mixed with anhydrous dimethylacetamide by solid-to-liquid ratio 1g/15mL, being heated to 65 DEG C makes hydroxypropyl
Methylcellulose dissolves, and is then hydroxypropyl first for the stearyl chloride and quality of 1.5 times of Hydroxypropyl methylcellulose to quality is added in solution
The triethylamine that 0.3 times of cellulose, vacuumizes stirring under inert gas shielding；Then solution is transferred in 35 DEG C of water-baths lazy
4h is reacted under property gas shield；Product is added in enough absolute ethyl alcohols after reaction is precipitated, depressurized after precipitation
Filter, takes solid and preliminary modified Hydroxypropyl methylcellulose is successively obtained after cleaning, drying；Preliminary modified hydroxypropyl first is fine
Dimension element is added in the glyoxal water solution that mass concentration is 8%, wherein the quality and second of preliminary modified Hydroxypropyl methylcellulose
20 times of glycol, the stirring reaction 1h at a temperature of 40 DEG C obtains twice-modified hypromellose after eventually passing washing, drying
Element.
A kind of preparation method of anti-oxidant heavy property aquatic products food calling particle, comprises the following steps：
1) preparation of core part：Each raw material is weighed by proportioning, each component is sieved respectively, and (phagostimulant crosses 200 mesh sieves, resists
Oxidation modification shell particles cross 40-80 mesh sieves, Hydroxypropyl methylcellulose, prominent release agent, retarding agent and cross 80 mesh sieves.Lubricant crosses 80 mesh
Sieve)；Anti-oxidant modified shell particles are added water and is stirred, be made the suspension that concentration is 10wt%, added under agitation
Enter the phagostimulant of 1/2 amount, adsorb 7h, after centrifugation, drying, obtain being adsorbed with the anti-oxidant modified shell particles of phagostimulant；Will be surplus
Remaining phagostimulant, the anti-oxidant modified shell particles for being adsorbed with phagostimulant, Hydroxypropyl methylcellulose, it is prominent release agent and be well mixed, will be viscous
Mixture ethanol dissolves；Granulated after above-mentioned well mixed raw material is mixed with adhesive, after drying, sieve grain, added
Mix lubricant is uniform.
2) preparation of shell：Each raw material is weighed by proportioning, each component is sieved respectively, and (phagostimulant crosses 200 mesh sieves, anti-oxidant
Modified shell particles cross 40-80 mesh sieves, Hydroxypropyl methylcellulose, prominent release agent, retarding agent and cross 80 mesh sieves.Lubricant crosses 80 mesh sieves)；Will
Anti-oxidant modified shell particles are added water and stir, and are made the suspension that concentration is 10wt%, and 1/2 amount is added under agitation
Phagostimulant, adsorb 7h, centrifugation, dry after, obtain being adsorbed with the anti-oxidant modified shell particles of phagostimulant；By remaining food calling
Agent, the anti-oxidant modified shell particles for being adsorbed with phagostimulant, Hydroxypropyl methylcellulose, retarding agent are well mixed, by adhesive second
Alcohol dissolves；By above-mentioned well mixed raw material and step 1) obtained by core part, adhesive granulated after being well mixed, then pass through
After dry, sieve grain, add mix lubricant uniform, finished product.
Embodiment 4
A kind of anti-oxidant heavy property aquatic products food calling particle, in hud typed.
Core part includes that the raw material of following weight portion is blended：55 parts of phagostimulant (SCFA), anti-oxidant change
Property 20 parts of shell particles, 17 parts of Hydroxypropyl methylcellulose (viscosity is 6000-10000mps), prominent release 3 parts of agent, adhesive (carboxymethyl
Sodium cellulosate) 4 parts, 1 part of lubricant (superfine silica gel powder).
Shell sections include that the raw material of following weight portion is blended：55 parts of phagostimulant (glycine betaine), anti-oxidant modified shellfish
17 parts of shell particle, 8 parts of Hydroxypropyl methylcellulose (viscosity is 6000-10000mps), 14 parts of retarding agent (ethyl cellulose), adhesive
3 parts of (sodium carboxymethylcellulose), 3 parts of lubricant (superfine silica gel powder)；The core part is 1 with the mass ratio of shell sections:4.
In the present embodiment,
The preparation method of the anti-oxidant modified shell particles is：
Shell is cleaned, is transferred in Muffle furnace, 1h is calcined at 400 DEG C；Cooling is taken out after roasting, shell is ground into
The shell particles of 40-80 mesh.
Weigh aluminium block, MAG block, spelter, and put into molten in the dilute nitric acid solution that excessive mass concentration is 25%
Solution, again to silver nitrate is added in solution after being completely dissolved, then adjusts pH to neutrality, obtains multiple metal ion solution, solution
The mol ratio of middle aluminium ion, magnesium ion, zinc ion and silver ion is 1.5:1.5:0.5:0.5；Multiple metal ion solution is existed
Stirred at 90 DEG C, to the shell particles that 1 times of solution quality is added in solution, be warming up to 110 DEG C, after standing adsorption 2h, taken
Go out shell particles, drying obtains anti-oxidant modified shell particles.
It is described it is prominent release agent preparation method be：
By quick lime powder and ethylene glycol in mass ratio 10:2 are mixed and stirred for uniformly, then the pressurized, heated at 130 DEG C
Stirring reaction 2h；The butyl lithium of quick lime powder quality 3% is added during 1h is reacted, reaction makes product cold after terminating
But to room temperature, it is obtained to dash forward and releases agent.
The Hydroxypropyl methylcellulose in the shell sections is by modification：
Hydroxypropyl methylcellulose is mixed with anhydrous dimethylacetamide by solid-to-liquid ratio 1g/20mL, being heated to 60 DEG C makes hydroxypropyl
Methylcellulose dissolves, and is then fine hydroxypropyl first for the stearyl chloride and quality of 1 times of Hydroxypropyl methylcellulose to quality is added in solution
The triethylamine of 0.2 times of dimension element, vacuumizes stirring under inert gas shielding；Then solution is transferred in 35 DEG C of water-baths in inertia
8h is reacted under gas shield；Product is added in enough absolute ethyl alcohols after reaction is precipitated, filtration under diminished pressure after precipitation,
Take solid and preliminary modified Hydroxypropyl methylcellulose is successively obtained after cleaning, drying；By preliminary modified hypromellose
Element is added in the glyoxal water solution that mass concentration is 7%, wherein the quality and second two of preliminary modified Hydroxypropyl methylcellulose
15 times of alcohol, the stirring reaction 2h at a temperature of 35 DEG C obtains twice-modified hypromellose after eventually passing washing, drying
Element.
A kind of preparation method of anti-oxidant heavy property aquatic products food calling particle, comprises the following steps：
1) preparation of core part：Each raw material is weighed by proportioning, each component is sieved respectively, and (phagostimulant crosses 200 mesh sieves, resists
Oxidation modification shell particles cross 40-80 mesh sieves, Hydroxypropyl methylcellulose, prominent release agent, retarding agent and cross 80 mesh sieves.Lubricant crosses 80 mesh
Sieve)；Anti-oxidant modified shell particles are added water and is stirred, be made the suspension that concentration is 15wt%, added under agitation
Enter the phagostimulant of 1/3 amount, adsorb 8h, after centrifugation, drying, obtain being adsorbed with the anti-oxidant modified shell particles of phagostimulant；Will be surplus
Remaining phagostimulant, the anti-oxidant modified shell particles for being adsorbed with phagostimulant, Hydroxypropyl methylcellulose, it is prominent release agent and be well mixed, will be viscous
Mixture ethanol dissolves；Granulated after above-mentioned well mixed raw material is mixed with adhesive, after drying, sieve grain, added
Mix lubricant is uniform.
2) preparation of shell：Each raw material is weighed by proportioning, each component is sieved respectively, and (phagostimulant crosses 200 mesh sieves, anti-oxidant
Modified shell particles cross 40-80 mesh sieves, Hydroxypropyl methylcellulose, prominent release agent, retarding agent and cross 80 mesh sieves.Lubricant crosses 80 mesh sieves)；Will
Anti-oxidant modified shell particles are added water and stir, and are made the suspension that concentration is 15wt%, and 1/3 amount is added under agitation
Phagostimulant, adsorb 8h, centrifugation, dry after, obtain being adsorbed with the anti-oxidant modified shell particles of phagostimulant；By remaining food calling
Agent, the anti-oxidant modified shell particles for being adsorbed with phagostimulant, Hydroxypropyl methylcellulose, retarding agent are well mixed, by adhesive second
Alcohol dissolves；By above-mentioned well mixed raw material and step 1) obtained by core part, adhesive granulated after being well mixed, then pass through
After dry, sieve grain, add mix lubricant uniform, finished product.
Food calling particle of the invention, the shelf-life is most long to be 1 year.
Food calling particle of the invention, after putting into clear water, can be maintained at water-bed or water body middle level.
Raw materials used in the present invention, equipment, unless otherwise noted, is the conventional raw material, equipment of this area；In the present invention
Method therefor, unless otherwise noted, is the conventional method of this area.
The above, is only presently preferred embodiments of the present invention, and not the present invention is imposed any restrictions, every according to the present invention
Any simple modification, change and equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side
The protection domain of case.
Claims (10)
1. a kind of anti-oxidant heavy property aquatic products food calling particle, it is characterised in that：Containing phagostimulant and as the food calling agent carrier
Anti-oxidant modified shell particles；The preparation method of the anti-oxidant modified shell particles is as follows：Aluminium block, MAG block, spelter are weighed,
And dissolving in excessive dilute nitric acid solution is put into, then adjust pH to silver nitrate is added in solution again after being completely dissolved
To neutral, multiple metal ion solution is obtained；Multiple metal ion solution is stirred at 85-95 DEG C, to adding in solution
Plus shell particles, 100-110 DEG C, after standing adsorption 1-2h is warming up to, shell particles are taken out, drying obtains anti-oxidant modified shell
Particle.
2. as claimed in claim 1 a kind of anti-oxidant heavy property aquatic products food calling particle, it is characterised in that the multiple metal ion
The mol ratio of aluminium ion, magnesium ion, zinc ion and silver ion is 0.5-1.5 in solution:0.5-1.5:0.5-1.5:0.5-1.5.
3. as claimed in claim 1 a kind of anti-oxidant heavy property aquatic products food calling particle, it is characterised in that the quality of the dust technology
Concentration is 20-40%.
4. as claimed in claim 1 a kind of anti-oxidant heavy property aquatic products food calling particle, it is characterised in that the matter of the shell particles
Measure is 0.5-1.5 times of multiple metal ion solution.
5. as claimed in claim 1 a kind of anti-oxidant heavy property aquatic products food calling particle, it is characterised in that the system of the shell particles
Preparation Method is：Shell is cleaned, is transferred in Muffle furnace, 1-2h is calcined at 300-400 DEG C；Cooling is taken out after roasting, by shellfish
Shell is ground into the shell particles of 40-80 mesh.
6. anti-oxidant heavy property aquatic products food calling particle as claimed in claim 5 a kind of, it is characterised in that the shell particles are also passed through
Overactivation treatment：It is the citric acid solution of 6-6.5 to prepare pH, and shell particles are soaked in the citric acid solution of its 8-12 times of quality
Bubble 3-5h, soaking temperature is 40-50 DEG C；Taken out after immersion, dried, obtain the shell particles of activation process.
7. as claimed in claim 1 a kind of anti-oxidant heavy property aquatic products food calling particle, it is characterised in that the aquatic products food calling particle
In hud typed, core part includes that the raw material of following weight portion is blended：Phagostimulant 45-55 parts, anti-oxidant modified shell
Grain 20-24 part, Hydroxypropyl methylcellulose 17-21 parts, dash forward release agent 3-5 parts, adhesive 2-4 parts, lubricant 1-3 parts；Shell sections bag
The raw material for including following weight portion is blended：Phagostimulant 45-55 parts, anti-oxidant modified shell particles 17-21 parts, hypromellose
It is plain 8-12 parts, retarding agent 14-18 parts, adhesive 2-4 parts, lubricant 1-3 parts；The core part and the mass ratio of shell sections
It is 1:4-10.
8. anti-oxidant heavy property aquatic products food calling particle as claimed in claim 7 a kind of, it is characterised in that the phagostimulant is selected from ammonia
One or more in base acid, nucleotides, glycine betaine, organic acid, SCFA；The retarding agent is ethyl cellulose；Institute
State one or more during adhesive is selected from polyvinylpyrrolidone, sodium carboxymethylcellulose；The lubricant be selected from talcum powder,
One or more in magnesium stearate, superfine silica gel powder.
9. as claimed in claim 7 a kind of anti-oxidant heavy property aquatic products food calling particle, it is characterised in that the prominent preparation for releasing agent
Method is：
By quick lime powder and ethylene glycol in mass ratio 10:2-3 is mixed and stirred for uniformly, and then pressurization adds at 130-140 DEG C
2-3h is reacted in thermal agitation；The butyl lithium of quick lime powder quality 3-4% is added during 0.5-1h is reacted, reaction makes after terminating
Product is cooled to room temperature, is obtained to dash forward and releases agent.
10. the preparation method of a kind of anti-oxidant heavy property aquatic products food calling particle as described in claim 1-9 is any, it is characterised in that
Comprise the following steps：
1) preparation of core part：Each raw material is weighed by proportioning, each component is sieved respectively；Anti-oxidant modified shell particles are added
Water is stirred, and is made the suspension that concentration is 5-15wt%, and the phagostimulant of 1/2-1/3 amounts, absorption are added under agitation
6-8h, after centrifugation, drying, obtains being adsorbed with the anti-oxidant modified shell particles of phagostimulant；By remaining phagostimulant, it is adsorbed with and lures
Eat the anti-oxidant modified shell particles of agent, Hydroxypropyl methylcellulose, it is prominent release agent and be well mixed, adhesive ethanol is dissolved；Will be upper
State and granulated after well mixed raw material mixes with adhesive, after drying, sieve grain, add mix lubricant uniform；
2) preparation of shell：Each raw material is weighed by proportioning, each component is sieved respectively；Anti-oxidant modified shell particles are added water and is stirred
Mix uniform, be made the suspension that concentration is 5-15wt%, the phagostimulant of 1/2-1/3 amounts is added under agitation, adsorb 6-8h,
After centrifugation, drying, obtain being adsorbed with the anti-oxidant modified shell particles of phagostimulant；By remaining phagostimulant, it is adsorbed with phagostimulant
Anti-oxidant modified shell particles, Hydroxypropyl methylcellulose, retarding agent be well mixed, adhesive ethanol is dissolved；Will be above-mentioned mixed
Close uniform raw material and step 1) obtained by core part, adhesive be well mixed after granulate, drying, sieve grain after, plus
Enter mix lubricant uniform, finished product.
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