CN108864323A - The extraction process of chitin in a kind of shrimp shell slag - Google Patents
The extraction process of chitin in a kind of shrimp shell slag Download PDFInfo
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- CN108864323A CN108864323A CN201810590498.XA CN201810590498A CN108864323A CN 108864323 A CN108864323 A CN 108864323A CN 201810590498 A CN201810590498 A CN 201810590498A CN 108864323 A CN108864323 A CN 108864323A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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Abstract
The invention discloses a kind of extraction processes of chitin in shrimp shell slag, belong to chitin extractive technique field, including：Step 1, separating treatment：Shrimp shell slag is squeezed into removal excessive moisture, the light-coloured vinegar aqueous solution that mass fraction is 25-50% is added into shrimp shell slag, is sufficiently stirred, separates shrimp shell with shrimp, forms the first mixture；Step 2, tepidarium processing：The first mixture obtained in step 1 is subjected to tepidarium processing, the temperature of processing is 45-55 DEG C, and the time of processing is 15-30min, obtains the second mixture；Step 3 takes off albumen processing；Step 4, decalcification processing；Step 5, decolorization；Step 6 is dried.The present invention is using remaining shrimp shell slag during production shrimp slurry as raw material chitin extraction, and the utilization of prawn shell slag is rationally and abundant, and the chitin extracted has the advantages that content of ashes is low, nitrogen content is low.
Description
Technical field
The present invention relates to chitin extractive technique field, more specifically, it relates to which chitin mentions in a kind of shrimp shell slag
Taking technique.
Background technique
Chitin is nontoxic, tasteless, biodegradable, not soluble in water, and crystallinity is high, but will obtain shell after its deacetylated processing
Glycan, with hydrophily, biological compatibility, antibiotic property is positively charged high molecular polymer.
Chitin and its derivative have antibacterial activity, and enhancing is immune, inhibits tumour, antiviral, reducing blood lipid and cholesterol,
Artery sclerosis is prevented and treated, hemoglutination promotes wound healing function, gastric acid inhibitory effect, a variety of lifes such as slow releasing carrier of medication function
Object activity and function, are widely used in biomaterial and field of medicaments, environment protection field, field of food industry, agriculture field
Etc..And chitin can be made into chitosan after deacetylated, to reach control cholesterol, inhibit bacterial activity, prevention
With control hypertension, adsorb and excrete the purpose of heavy metal, added value is higher.
In marine product production process, it will usually some slag charges occur, if shrimps are when producing shrimp slurry or shrimp cream, be centrifuged
It is inevitably generated shrimp shell slag in process, and contains shrimp shell and a small amount of shrimp in shrimp shell slag, if shrimp shell slag is directly lost
It abandons, easily causes the waste of raw material, and contain chitin in shrimp shell slag, if being extracted, not only only help to the conjunction of material
Reason utilizes, and additionally aids to form high value-added product, to promote the production class of company.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of extraction work of chitin in shrimp shell slag
Skill has the advantages that rationally to utilize shrimp shell slag and extracts chitin.
To achieve the above object, the present invention provides following technical solutions：
The extraction process of chitin, includes the following steps in a kind of shrimp shell slag：
Step 1, separating treatment：Shrimp shell slag is squeezed into removal excessive moisture, it is 25-50%'s that mass fraction is added into shrimp shell slag
Light-coloured vinegar aqueous solution, is sufficiently stirred, and separates shrimp shell with shrimp, forms the first mixture；
Step 2, tepidarium processing：The first mixture obtained in step 1 is subjected to tepidarium processing, the temperature of processing is
45-55 DEG C, the time of processing is 15-30min, obtains the second mixture；
Step 3 takes off albumen processing：It is 3-5%'s that excessive mass fraction will be added in the second mixture obtained in step 2
NaOH solution is sufficiently stirred, and obtains de- protein mixture；
Step 4, decalcification processing：It is 2-3%'s that excessive mass fraction is added in the de- protein mixture obtained into step 3
HCl solution, stirring stand 1.5-2h, and washing, obtaining pH value is neutral decalcification mixture；
Step 5, decolorization：Hydrogen peroxide is added in the decalcification mixture obtained into step 4, stirs, obtains the first of white
The mixture of shell element and hydrogen peroxide；
Step 6 is dried：The mixture of the chitin obtained in step 5 and hydrogen peroxide is dry through heat drying, obtain white
Chitin powder.
Through the above technical solutions, being impregnated using light-coloured vinegar aqueous solution prawn shell slag in step 1, disinfection can be played
Effect, at the same time it can also soften shrimp shell and shrimp.In conjunction with the effect of stirring, easily separate shrimp shell with shrimp, and then after making
When continuous operation, shrimp shell can occur adequately to contact with corresponding reaction medium respectively with shrimp, so that the yield of extraction is improved, and
And the time needed for reducing production.
In step 2, the first mixture is subjected to tepidarium processing, helps speed up the volatilization of light-coloured vinegar, through the above-mentioned time and
At a temperature of tepidarium processing after, the light-coloured vinegar content in the second mixture of acquisition is extremely low.
In step 3, above-mentioned NaOH solution is added, can make NaOH solution to the full extent prawn shell and shrimp carry out compared with
The effect of good deproteination, and then keep the purity of the de- protein mixture obtained higher.
In step 4, the addition of HCl solution helps that neutralization reaction occurs with NaOH solution remaining in step 3, and
Excessive HCl solution can react with the calcium substance in shrimp shell, shrimp, to reach preferable decalcification.
In step 5, hydrogen peroxide has the function of preferably to decolourize, and chitin can be become to white.
In step 6, dry processing, hydrogen peroxide volatilization, the remaining higher chitin powder of purity are dried through overheat.
To sum up, by the extraction process in the application, the purity of the chitin of acquisition is higher, and quality is preferable.
Further preferably：In the step 1, shrimp shell slag, which is placed in agitating device, to be stirred, the agitating device packet
Include autoclave body, lid, the feed inlet being opened on lid, the mixing part being set on lid and the electricity of driving mixing part movement
Machine；The mixing part includes shaft, the first stirring parts, the second stirring parts, is set in shaft and is used to while controlling first stir
Mix part and actuator that the second stirring parts are rotated in the opposite sense, the shaft is connected to motor, and first stirring parts and drives
Moving part connection, second stirring parts are fixedly connected with shaft.
Through the above technical solutions, shaft drives the first stirring parts to rotate in one direction when electric motor starting, first is realized
The stirring action of stirring parts；And the rotation of shaft, driving the second stirring parts rotates backward, and realizes that the stirring of the second stirring parts is made
With.The mixing direction of first stirring parts and the second stirring parts helps to save point on the contrary, therefore, the mixing effect reached is more preferable
From required time.
Further preferably：The actuator includes first bevel gear, second bevel gear, third hand tap gear, fixed block；Institute
It states first bevel gear, third hand tap gear described in bevel gear to be arranged in parallel, the third gear is bored with first bevel gear, third respectively
Gear engagement；The first bevel gear is placed on outside shaft and is fixedly connected with shaft；The second bevel gear and fixed block are solid
Fixed connection, the shaft is across second bevel gear and fixed block and the second bevel gear and shaft, fixed block and shaft
Between be respectively arranged with bearing, the fixed block is arranged on lid；The third hand tap gear is set to autoclave body by support rod
On.
Through the above technical solutions, first bevel gear can be driven to be rotate in same direction together when shaft rotates, and third is bored
Gear is engaged with first bevel gear and second bevel gear simultaneously, and between second bevel gear and shaft, between fixed block and shaft
It is respectively arranged with bearing, therefore, first bevel gear can drive third hand tap gear to rotate, then drive the second cone tooth by third hand tap gear
Wheel rotation, it is final drive fixed block and the second stirring parts connect with fixed block along the opposite direction rotated with first bevel gear into
Row rotation realizes that the reverse agitating function of the first stirring parts and the second stirring parts moves.
Further preferably：First stirring parts include first horizontal plate and are arranged with level board integrally connected
Vertical plate, the first horizontal plate are fixedly connected with fixed block.
Through the above technical solutions, when the spindle is rotated, driving first horizontal plate and vertical plate to rotate together, vertical plate inclines
It is tiltedly connected on first horizontal plate, resistance can be increased in whipping process, to keep stirring more effect more obvious.Further
Preferably：Second stirring parts include the stirring structure of the lantern-shaped on second horizontal plate and fixation and second horizontal plate,
The agitating paddle includes several curved stirring rods.
Through the above technical solutions, several curved stirring rods, both ends are respectively fixedly connected with, to form lantern-shaped
Stirring structure, and there is gap between adjacent stirring rod, during the stirring of the second stirring parts, stirring structure be can contact
The mixture that larger range of shrimp shell slag and light-coloured vinegar aqueous solution are formed, the mixing effect for playing the second stirring parts are more preferable.Into one
Step is preferably：In the step 1, the speed of stirring is 60-80rpm, and the time of stirring is 30-45min.
Through the above technical solutions, using above-mentioned mixing speed and mixing time, can energy saving to the full extent, and
And it equally can achieve the effect of preferable shrimp shell, shrimp separation.
Further preferably：After the washing of the step 4, lemon juice, the volume of lemon juice and decalcification mixture is added
Than for 20-30:1, it is sufficiently stirred, stands 1-2min, wash again, until the pH value of the decalcification mixture obtained is neutrality.
Through the above technical solutions, lemon juice has pure and fresh smell, it can remove fishy smell, the lemon of above-mentioned volume ratio be added
After juice, the fishy smell in de- protein mixture can be effectively removed, goes the fishy smell in the chitin powder finally obtained almost
It removes.
Further preferably：In the step 4, the volume ratio of HCl solution and de- protein mixture is 2-3.5:1.
Through the above technical solutions, HCl solution requires to be excessively used, and in above-mentioned volume ratio range, the dosage of HCl solution
Although excessive, using the HCl solution and de- protein mixture of above-mentioned volume ratio range, help to save to a certain extent and mention
Take cost.
Further preferably：In the step 5, the volume ratio of hydrogen peroxide and deodorization mixture is 1.5-3.5:1, in 40-
It is stirred in 45 DEG C of water bath.
Through the above technical solutions, hydrogen peroxide within the scope of aforementioned proportion, can adequately decolourize to deodorization mixture
Effect, and
Further preferably：In the step 7, it is 70-75 DEG C that heat, which dries dry temperature,.
Through the above technical solutions, the drying of progress heat is dry within the said temperature range, on the one hand sufficiently it can dry and obtain
On the other hand chitin powder can sufficiently remove hydrogen peroxide.
In conclusion the invention has the advantages that：
1. with being compared using shrimp as raw material, cost is lower, without being removed the step such as shrimp line using shrimp shell slag as raw material
Suddenly, easy to operate；
2. remaining shrimp shell slag prepares chitin as raw material after being treated as the discarded preparation shrimp slurry of slag charge originally, eventually
Value-added content of product improves, and the class of company's production product also gets a promotion；
3. being in the light-coloured vinegar aqueous solution of 25-50% by the mass fraction that shrimp shell slag is placed in light-coloured vinegar, stirring of going forward side by side helps to improve shrimp
The separating effect of shell and shrimp, convenient for that shrimp shell can be made to come into full contact with the molten of corresponding addition with shrimp in de- albumen, decalcification processing
Liquid.
Detailed description of the invention
Fig. 1 is the flow diagram of the extraction process of chitin in shrimp shell slag in embodiment 1；
Fig. 2 be in embodiment 1 in shrimp shell slag in the extraction process of chitin agitating device structural schematic diagram；
Fig. 3 be in embodiment 1 in shrimp shell slag in the extraction process of chitin agitating device structural schematic diagram, be mainly used for embodying
Shaft, first bevel gear, second bevel gear, the structure of third hand tap gear；
Fig. 4 be in embodiment 1 in shrimp shell slag in the extraction process of chitin agitating device structural schematic diagram, be mainly used for embodying
First stirring parts, the second stirring parts, the structure of fixed block.
In figure, 1, autoclave body；2, lid；3, feed inlet；4, mixing part；41, shaft；42, the first stirring parts；421, the first water
Plate；422, vertical plate；43, the second stirring parts；431, second horizontal plate；432, stirring rod；441, first bevel gear；442,
Two bevel gears；443, third hand tap gear；444, fixed block；5, motor；6, support rod；7, bearing；8, discharge port；9, through-hole.
Specific embodiment
With reference to the accompanying drawings and examples, the present invention will be described in detail.
Embodiment 1：The extraction process of chitin in a kind of shrimp shell slag, as shown in Figure 1, acquisition is made by the steps：
Step 1, separating treatment：By shrimp shell slag squeeze removal excessive moisture, into shrimp shell slag be added mass fraction be 35% it is white
Diluted vinegar solution stirs 40min with the speed of 70rpm, separates shrimp shell with shrimp, forms the first mixture；
Step 2, tepidarium processing：The first mixture obtained in step 1 is subjected to tepidarium processing, the temperature of processing is 50
DEG C, the time of processing is 25min, obtains the second mixture；
Step 3 takes off albumen processing：It is 4% that excessive mass fraction will be added in the second mixture obtained in step 2
NaOH solution is sufficiently stirred, and obtains de- protein mixture；
Step 4, decalcification processing：It is molten that the HCl that mass fraction is 2.5% is added in the de- protein mixture obtained into step 3
The volume ratio of liquid, HCl solution and de- protein mixture is 2.5:1, stirring stands 2h, and washing, obtaining pH value is neutral decalcification
Mixture；
Step 5, decolorization：Hydrogen peroxide, hydrogen peroxide and deodorization mixture are added in the decalcification mixture obtained into step 4
Volume ratio be 2:1, it is stirred in 45 DEG C of water bath, obtains the chitin of white and the mixture of hydrogen peroxide；
Step 6 is dried：By the mixture of the chitin obtained in step 5 and hydrogen peroxide, heat is dried in the environment of 75 DEG C
It is dry, obtain the chitin powder of white.
Wherein, the agitating device in step 1, as shown in Fig. 2, including autoclave body 1, lid 2, the charging being opened on lid 2
Mouth 3 and the discharge port 8 for being opened in 1 bottom of autoclave body.
Referring to Fig. 3, a circular through-hole 9 is offered on lid 2, a motor 5 is provided with above through-hole 9, and
The shaft 41 for passing through through-hole 9 is connected on motor 5.On the part that shaft 41 is exposed to lid 2, level is arranged with one
First bevel gear 441, the first bevel gear 441 and shaft 41 are welded.In shaft 41 below first bevel gear 441, it is arranged
There are second bevel gear 442 and columnar fixed block 444（Referring to Fig. 4）, fixed block 444 is welded in the lower end of second bevel gear 442
On face, and between second bevel gear 442 and shaft 41, between fixed block 444 and shaft 41, carried out respectively by two bearings 7
Connection（In conjunction with Fig. 3 and Fig. 4）；In addition, second bevel gear 442 is located at the top of through-hole 9, fixed block 444 passes through through-hole 9（Reference
Fig. 4）.
Pass through the branch being horizontally fixed on metope in the side of first bevel gear 441 and second bevel gear 442 referring to Fig. 3
Strut 6 is provided with a third hand tap gear 443, and third hand tap gear 443 respectively with first bevel gear 441, second bevel gear 442
Engagement.
Referring to Fig. 4, in the lower end of fixed block 444, horizontal symmetrical is welded with four first horizontal plates 421, at every first
It is tiltedly staggered respectively on level board 421 and is welded with a vertical plate 422.
Referring to Fig. 4, in the shaft 41 below lid 2, horizontal symmetrical is welded with two pieces of second horizontal plates 431, at every piece
On an end on second horizontal plate 431 far from shaft 41, it is welded with the stirring structure of a lantern-shaped, which includes
The two ends correspondence of the stirring rod 432 of 14 bending cambers, every stirring rod 432 is welded together to form lantern-shaped.
Embodiment 2：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, in step 1, add
Enter the light-coloured vinegar aqueous solution that mass fraction is 25%, 40min is stirred with the speed of 80rpm.
Embodiment 3：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, in step 1, add
Enter the light-coloured vinegar aqueous solution that mass fraction is 50%, 30min is stirred with the speed of 60rpm.
Embodiment 4：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, in step 2, temperature
The temperature of water bath processing is 45 DEG C, and the time of processing is 30min.
Embodiment 5：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, in step 2, temperature
The temperature of water bath processing is 55 DEG C, and the time of processing is 15min.
Embodiment 6：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, in step 3,
The mass fraction of NaOH solution is 3%.In step 4, when decalcification is handled, the mass fraction of HCl is 2% in HCl solution, is stood
1.5h, washing.
Embodiment 7：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, in step 3,
The mass fraction of NaOH solution is 5%.In step 4, when decalcification is handled, the mass fraction of HCl is 3% in HCl solution, stands 2h,
Washing.
Embodiment 8：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, the washing of step 4
Later, the volume ratio of addition lemon juice, lemon juice and decalcification mixture is 20:1, it is sufficiently stirred, stands 2min, wash again,
Until the pH value of the decalcification mixture obtained is neutrality.
Embodiment 9：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, the washing of step 4
Later, the volume ratio of addition lemon juice, lemon juice and decalcification mixture is 25:1, it is sufficiently stirred, stands 1.5min, again water
It washes, until the pH value of the decalcification mixture obtained is neutrality.
Embodiment 10：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, the water of step 4
After washing, lemon juice is added, the volume ratio of lemon juice and decalcification mixture is 30:1, it is sufficiently stirred, stands 1min, again water
It washes, until the pH value of the decalcification mixture obtained is neutrality.
Embodiment 11：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, it is double in step 5
The volume ratio of oxygen water and deodorization mixture is 1.5:1, it is stirred in 40 DEG C of water bath.
Embodiment 12：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, it is double in step 5
The volume ratio of oxygen water and deodorization mixture is 3.5:1, it is stirred in 45 DEG C of water bath.
Comparative example 1：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, it is white in step 1
The mass fraction of light-coloured vinegar is 20% in diluted vinegar solution.
Comparative example 2：The extraction process of chitin in a kind of shrimp shell slag, the difference from embodiment 1 is that, in step 1, adopt
With application No. is the blenders in CN201510241861.3 to be stirred.
Test one：Yield test
Test specimen：The chitin that the technique of selection embodiment 1-12 extracts chooses comparative example 1-2's as test sample 1-12
The chitin that technique extracts is opposed 1-2 in the same old way.
Test method：
1. the quality of the shrimp shell slag after extruding excessive moisture in the step of embodiment 1-12, comparative example 1-2 one is weighed, remember
For m1, the weight by embodiment 1-12, comparative example the 1-2 chitin finally obtained is m2, calculates chitin in each technique
Yield, record and analyze；
2. the smell of light olfactory test sample 1-12, record.
Test result：The yield of chitin is as shown in table 1 in embodiment 1-12, comparative example 1-2；The smell of test sample 1-12
As shown in table 2.
The yield of chitin in 1 embodiment 1-12 of table, comparative example 1-3
As shown in Table 1, the yield of chitin is higher in embodiment 1-12, but the yield of comparative example 1-2 chitin obtained compared with
It is low, illustrate during the extraction process, the combination of the mass fraction, the mixing effect of agitating device of light-coloured vinegar in light-coloured vinegar aqueous solution, to first
The yield of shell element will cause large effect.
The smell of 2 test sample 1-12 of table
As shown in Table 2, test sample 8-10 then has fishy smell without fishy smell, other test specimens, then after the washing for illustrating step 4,
Lemon juice is added, the fishy smell in chitin can be effectively removed.
Test two：Ash content detection test
Test specimen：The chitin that the technique of selection embodiment 1-12 extracts chooses comparative example 1-2's as test sample 1-12
The chitin that technique extracts is opposed 1-2 in the same old way.
Test method：By crucible with 1:10min is boiled in boiling water after 5 HCl impregnates, cleans to be put into drying box and dry,
It places into Muffle furnace, temperature setting is 550 DEG C, calcination 30min, is put into the dry cooling of drying box after taking out the cooling 1min of room temperature
30min, it is rear to be weighed using high accuracy balance rapidly, record data.Then it repeats the above steps, until weighing record twice in succession
Data differ less than 0.002g, quality at this time is constant, records the weight of crucible at this time, is denoted as m0。
Test sample 1-12, control sample 1-3 are dried in vacuo, the repeatedly dry weighing of a certain amount of chitin is taken, until weighing
2 differences are less than 0.002g before and after quality, it is therefore an objective to remove the moisture in test sample 1-12, control sample 1-3.Accurately weigh
2.00g dry chitin sample, is put into the crucible for having reached constant weight, first on electric jacket slow heating charing to smokeless,
It is then placed in Muffle furnace, is warming up to 550 DEG C, calcination 4h, be down to 200 DEG C of taking-ups to furnace temperature, be put into after the cooling 1min of room temperature dry
The dry cooling 30min of dry case, weighing record data.550 DEG C of calcination 1h in Muffle furnace are put into after weighing herein, cool down, is dry,
Weighing records data at this time, the as quality and m of crucible and ash content to 2 weight differences less than 0.002g2。
It calculates：Content of ashes is indicated in food with quality percentage：
Wherein, m0--- the quality of crucible；
m1--- chitin sample quality（2.00g）；
m2--- the quality of ash content and crucible after chitin sample calcination and.
Test result：Content of ashes in test sample 1-12, control sample 1-2 is as shown in table 3.
Content of ashes in 3 test sample 1-12 of table, control sample 1-2
As shown in Table 3, the content of ashes in test sample 1-12 is lower, floats in the range of 1.6-1.7%, and in control sample 1-2
Content of ashes it is then higher, beyond as defined in industrial grade standard≤2%, above situation explanation, during pretreated, light-coloured vinegar
The addition of aqueous solution, stirring whether sufficiently and in the HCl solution of addition HCl mass percentage, can be to the sample of acquisition
Content of ashes in product impacts, i.e.,：It is more abundant to the separation of shrimp shell in raw material and shrimp in the early period of extraction process, have
Help the probability come into full contact with for improving it with HCl solution, decalcification effect more preferably, so that the ash content in the chitin obtained be made to contain
It measures lower.
Test three：The detection of nitrogen content is tested
Test specimen：The chitin that the technique of selection embodiment 1-12 extracts chooses comparative example 1-3's as test sample 1-12
The chitin that technique extracts is opposed 1-3 in the same old way.
Test method：
1. preparation of reagents
Mixed indicator：Methyl red-ethanol solution：0.1g methyl red adds tri-distilled water to be settled to 100ml；Bromocresol green-ethyl alcohol is molten
Liquid：0.5g bromocresol green is settled to 100ml after being dissolved in tri-distilled water, and the used time mixes the two in equal volume, ready-to-use.
Boric acid solution：2.0g boric acid adds tri-distilled water to dissolve and is settled to 100ml, and 2% boric acid solution is made.
NaOH solution：40.0gNaOH is settled to 100ml, is configured to 40% NaOH solution.
HCl standard solution：The dense HCl of 1ml is taken to add water to 240ml
All reagents are all made of the tri-distilled water without ammonia and other ions and prepare.
2. operating method accurately weighs 0.5g test specimen, its is moved into clean and dry 500ml after finely ground respectively and is determined
In nitrogen bottle, it is separately added into 0.9g copper sulphate, 15g anhydrous potassium sulfate, 25mL sulfuric acid, is uniformly mixed, by bottle with the oblique Zhi Yuyou of 45° angle
On the asbestos gauge of aperture, small fire heating after foam completely disappears, reinforces firepower, and keep in bottle until content all carbonizes
Liquid it is slightly boiled and clarification it is dark green after, be further continued for heating 2h.
Nitrogen fixing bottle is removed, after letting cool, 200mL tri-distilled water is carefully added into, shakes up, then be carefully slowly added into 100ml along bottle wall
The NaOH solution that mass fraction is 40%, installs rapidly distilling apparatus, stoppers the rodlike glass plug of small glass cup, clamps screw clamp, to prevent
Gas leakage.
50mL20g/L boric acid solution and mixed indicator are added into receiving bottle（0.1% methyl red-ethanol solution and 0.5%
Bromocresol green-ethanol solution mixes in equal volume）Few drops, and condenser pipe lower end is made to be inserted into liquid level 1cm or less.
After beginning to warm up distillation, steam is passed through reaction chamber, and ammonia is entered in receiving bottle by condenser pipe, distills 5min.It moves
Dynamic receiving bottle, makes condenser pipe lower end leave liquid level, distills 1min, is then rinsed outside condenser pipe lower end with a small amount of water.It removes and connects
Bottle is received, stops heating distillation, with HCl standard solution（0.05mol/L）Titration, solution become bois de rose from blue-green to titrate eventually
Point.
Weigh 0.1g glucose（It analyzes pure）, instead of test specimen, copper sulphate, the sulfuric acid of equivalent are added according to the method described above
Potassium and sulfuric acid distill after digestion, as blank group, HCl titer volume required for record titrates.The volume of consumption can not be big
In 0.3ml, otherwise to be unreasonable as a result, it is desirable to re-operate and titrate.
3. calculating：
X --- nitrogen content in sample（%）；
V1--- the volume of HCl standard solution is consumed when titration sample（mL）；
V2--- the volume of titration blank reagent consumption HCl standard solution（mL）；
C --- the concentration of HCl standard solution（mol/L）；
0.014——HCl（cHCl=1.0mol/L）The quality of comparable nitrogen in standard solution（g）；
The quality of m --- sample（g）.
Test result：Nitrogen content in test sample 1-12, control sample 1-2 is as shown in table 4.
Nitrogen content in 4 test sample 1-12 of table, control sample 1-2
As shown in Table 4, the nitrogen content in test sample 1-12 is lower, floats in the range of 6.8-6.9%, and in control sample 1-2
Content of ashes is then higher, and more than 7.5%, above situation explanation, during pretreated, addition, the stirring of light-coloured vinegar aqueous solution are
The mass percentage of NaOH, can cause the nitrogen content in the sample of acquisition in no abundant and addition NaOH solution
It influences, i.e.,：It is more abundant to the separation of shrimp shell in raw material and shrimp in the early period of extraction process, it is molten with NaOH to help to improve it
The probability of liquid come into full contact with, Deproteinated better effect, to keep the nitrogen content in the chitin obtained lower.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. the extraction process of chitin in a kind of shrimp shell slag, which is characterized in that include the following steps：
Step 1, separating treatment：Shrimp shell slag is squeezed into removal excessive moisture, it is 25-50%'s that mass fraction is added into shrimp shell slag
Light-coloured vinegar aqueous solution, is sufficiently stirred, and separates shrimp shell with shrimp, forms the first mixture；
Step 2, tepidarium processing：The first mixture obtained in step 1 is subjected to tepidarium processing, the temperature of processing is
45-55 DEG C, the time of processing is 15-30min, obtains the second mixture；
Step 3 takes off albumen processing：It is 3-5%'s that excessive mass fraction will be added in the second mixture obtained in step 2
NaOH solution is sufficiently stirred, and obtains de- protein mixture；
Step 4, decalcification processing：It is 2-3%'s that excessive mass fraction is added in the de- protein mixture obtained into step 3
HCl solution, stirring stand 1.5-2h, and washing, obtaining pH value is neutral decalcification mixture；
Step 5, decolorization：Hydrogen peroxide is added in the decalcification mixture obtained into step 4, stirs, obtains the first of white
The mixture of shell element and hydrogen peroxide；
Step 6 is dried：The mixture of the chitin obtained in step 5 and hydrogen peroxide is dry through heat drying, obtain white
Chitin powder.
2. the extraction process of chitin in a kind of shrimp shell slag according to claim 1, which is characterized in that the step 1
In, shrimp shell slag, which is placed in agitating device, to be stirred, and the agitating device includes autoclave body, lid, the charging being opened on lid
The motor of mouth, the mixing part being set on lid and the movement of driving mixing part；The mixing part includes shaft, the first stirring
Part, the second stirring parts are set in shaft and are used to while controlling the first stirring parts be rotated in the opposite sense with the second stirring parts
Actuator, the shaft is connected to motor, and first stirring parts are connect with actuator, and second stirring parts and shaft are solid
Fixed connection.
3. the extraction process of chitin in a kind of shrimp shell slag according to claim 2, which is characterized in that the actuator packet
Include first bevel gear, second bevel gear, third hand tap gear, fixed block；First bevel gear described in the bevel gear, third hand tap gear
It is arranged in parallel, the third gear is engaged with first bevel gear, third hand tap gear respectively；The first bevel gear is placed on outside shaft
Portion is simultaneously fixedly connected with shaft；The second bevel gear is fixedly connected with fixed block, and the shaft is across second bevel gear and admittedly
Determine between block and the second bevel gear and shaft, be respectively arranged with bearing between fixed block and shaft, the fixed block is worn
In on lid；The third hand tap gear is set on autoclave body by support rod.
4. the extraction process of chitin in a kind of shrimp shell slag according to claim 2, which is characterized in that first stirring
Part includes that first horizontal plate and the vertical plate with the setting of level board integrally connected, the first horizontal plate are fixed with fixed block
Connection.
5. the extraction process of chitin in a kind of shrimp shell slag according to claim 5, which is characterized in that second stirring
Part includes the stirring structure of the lantern-shaped on second horizontal plate and fixation and second horizontal plate, and the agitating paddle includes several
Curved stirring rod.
6. the extraction process of chitin in a kind of shrimp shell slag according to claim 1, which is characterized in that the step 1
In, the speed of stirring is 60-80rpm, and the time of stirring is 30-45min.
7. the extraction process of chitin in a kind of shrimp shell slag according to claim 1, which is characterized in that the step 4
After washing, lemon juice is added, the volume ratio of lemon juice and decalcification mixture is 20-30:1, it is sufficiently stirred, stands 1-2min,
It washes again, until the pH value of the decalcification mixture obtained is neutrality.
8. the extraction process of chitin in a kind of shrimp shell slag according to claim 1, which is characterized in that the step 4
In, the volume ratio of HCl solution and de- protein mixture is 2-3.5:1.
9. the extraction process of chitin in a kind of shrimp shell slag according to claim 1, which is characterized in that the step 5
In, the volume ratio of hydrogen peroxide and deodorization mixture is 1.5-3.5:1, it is stirred in 40-45 DEG C of water bath.
10. the extraction process of chitin in a kind of shrimp shell slag according to claim 1, which is characterized in that the step 7
In, it is 70-75 DEG C that heat, which dries dry temperature,.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110699276A (en) * | 2019-09-30 | 2020-01-17 | 广西民族大学 | Strain of chitin-like paenibacillus and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0542249A3 (en) * | 1991-11-13 | 1994-08-10 | Shinetsu Chemical Co | Method for preparing chitosan |
| CN104277141A (en) * | 2014-10-28 | 2015-01-14 | 陈冬年 | Method for extracting chitin from dried shrimp shells |
| CN104877043A (en) * | 2015-06-06 | 2015-09-02 | 淮海工学院 | Method of extracting chitin in crab shell powder |
| CN107602712A (en) * | 2017-10-31 | 2018-01-19 | 吴宇 | A kind of Starch Production raw material cleaning device |
| CN207012961U (en) * | 2017-04-18 | 2018-02-16 | 现代（三河）工程塑料有限公司 | A kind of well-mixed highly effective reaction kettle of solid-liquid |
-
2018
- 2018-06-09 CN CN201810590498.XA patent/CN108864323A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0542249A3 (en) * | 1991-11-13 | 1994-08-10 | Shinetsu Chemical Co | Method for preparing chitosan |
| CN104277141A (en) * | 2014-10-28 | 2015-01-14 | 陈冬年 | Method for extracting chitin from dried shrimp shells |
| CN104877043A (en) * | 2015-06-06 | 2015-09-02 | 淮海工学院 | Method of extracting chitin in crab shell powder |
| CN207012961U (en) * | 2017-04-18 | 2018-02-16 | 现代（三河）工程塑料有限公司 | A kind of well-mixed highly effective reaction kettle of solid-liquid |
| CN107602712A (en) * | 2017-10-31 | 2018-01-19 | 吴宇 | A kind of Starch Production raw material cleaning device |
Non-Patent Citations (4)
| Title |
|---|
| SONG, YONG-SU 等: "Extraction of chitin and chitosan from larval exuvium and whole body of edible mealworm, Tenebrio molitor", 《ENTOMOLOGICAL RESEARCH》 * |
| 刘宏喜: "蚝壳甲壳素的提取及其衍生物在印染中的应用", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 别尔林: "《有机化学实验操作技术》", 31 May 1963, 中国工业出版社 * |
| 高志敏: "《厨房小窍门新编》", 31 August 2002, 中国电力出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110699276A (en) * | 2019-09-30 | 2020-01-17 | 广西民族大学 | Strain of chitin-like paenibacillus and application thereof |
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Address after: 317607 No.9 Jiusheng Road, bingang industrial city, Yuhuan City, Taizhou City, Zhejiang Province Applicant after: Zhejiang Yifeng marine biologicals Co., Ltd. Address before: 317607 Si Bian village, Sha Men town, Yuhuan County, Taizhou, Zhejiang Applicant before: Zhejiang Yifeng marine biologicals Co., Ltd. |
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Application publication date: 20181123 |