CN108003636A - A kind of preparation method of antibacterial heat resistant type gelatin - Google Patents
A kind of preparation method of antibacterial heat resistant type gelatin Download PDFInfo
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Abstract
The present invention relates to gelatin preparing technical field, and in particular to a kind of preparation method of antibacterial heat resistant type gelatin.The present invention is to make gelatin base substrate by oneself as matrix,Modified sodium alginate,Chitin nano fiber and silver nitrate solution are made by oneself as reinforcing agent,And it is aided with chitosan,Antibacterial heat resistant type gelatin is prepared in Geniposide and ethylenediamine etc.,Fish-skin is handled first with acid-base solution to obtain self-control gelatin base substrate,Sodium metaperiodate is recycled to be modified sodium alginate,Interacted using the hydrogen bond in chitin nano fiber and chitosan molecule,The mechanical property for being conducive to gelatin is improved,It is subsequently added into chitosan,The semi-interpenetrating polymer network structure of formation upsets the normal physiological activity of bacterial cell,So as to reach the effect for killing bacterium,Matrix is modified using silver nitrate solution,Realize durable antibiotic,It is eventually adding Geniposide,The inierpeneirating network structure of formation can bear larger external force,Further improve the mechanical property of gelatin,It is with a wide range of applications.
Description
Technical field
The present invention relates to gelatin preparing technical field, and in particular to a kind of preparation method of antibacterial heat resistant type gelatin.
Background technology
Extract of the gelatin as animal collagen tissue, is a kind of natural polymer and biological macromolecule material.It is bright
Glue is also a kind of higher low-calorie health food of nutritive value, can be used for making additive of candy, frozen food additive etc..
It has good biocompatibility, no antigen, hemostasis and promotes the performances such as organization healing, and therefore, gelatin is also by extensive profit
Use in medicine and chemical industry.The gelatin resources reserve in China is enriched, derived from a wealth of sources, is cheap, and since gelatin is good
The performance such as reactivity, film forming, coagulability, biocompatibility, degradability, green environmental protection and recyclability, make it
Become the research hotspot of biological macromolecule material scientific domain in recent years.
At present, more than 90% gelatin derives from pig, the skin and bone of ox in the world, but due to fearing to rabid ox disease, aftosa
Reason, the applications of mammal gelatin such as flurried and religious belief receive certain limitation.Research finds, isinglass have with
The similar gelation of mammal gelatin, can be as a kind of material of new replacement mammal gelatin.
In recent years, some national research institutions utilize fish-skin, fish scale, the fish-bone extraction gelatin in fish accessory substance.But
Since the living environment temperature of fish is less than mammal, its gelling performance of gelatin and heat for being prepared using fish-skin, fish scale as raw material
Stability is relatively poor, and fish collagen is more degradable compared with pig, cow leather collagen, therefore is produced using these methods
Fish gelatin including gelling performance etc. property not as good as pig, cattle hide gelatin, as a result cause fish gelatin product to push away in practice
Wide application is restricted.
It is many to improve the functional characteristic method of isinglass, such as electrostatic method, enzyme process, chemical method.But fish prepared by electrostatic method
Gelatin properties are unstable, the phenomenon being separated easily occur；Enzyme process does not ensure that the gel strength and thermal stability of isinglass
It is completely the same；Chemical method is readily incorporated new harmful substance.
Therefore, developing a kind of gelatin that can solve above-mentioned performance issue is highly desirable.
The content of the invention
The technical problems to be solved by the invention：For common gelatin at present there are antibiotic property is poor, poor mechanical property and
Heat endurance is poor, the defects of can not meet market demands, there is provided a kind of preparation method of antibacterial heat resistant type gelatin.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of antibacterial heat resistant type gelatin, it is characterised in that specifically preparation process is：
（1）Weigh 10~12g sodium alginates and pour into the beaker with 24~32mL absolute ethyl alcohols and be mixed, it is outstanding to obtain self-control
Supernatant liquid, then weigh 6~8g sodium metaperiodates and pour into the beaker with 32~36mL deionized waters and be mixed, obtain making by oneself molten
Liquid, self-control solution is added in above-mentioned self-control suspension, and reaction is mixed at room temperature unglazed, obtains reaction solution, continues
Reaction is mixed in the ethylene glycol that reaction solution volume 3% is added into reaction solution, mixed liquor is obtained, by mixed liquor and absolute ethyl alcohol
It is mixed, filters and remove filtrate, wash filter residue with absolute ethyl alcohol, finally the filter residue after washing is put into surface plate, by table
Face ware is placed in drying in baking oven, obtains modified sodium alginate；
（2）Weigh 0.4~0.6kg crab shells and pour into 0.6~0.8L deionized waters and soak, immersion, which is placed in baking oven, dries, and dries
120 mesh sieves are crossed after crab shell is ground after dry, collect sieving crab shell powder, sieving crab shell powder and mixed in hydrochloric acid are placed in burning
It is mixed in cup, is put into centrifuge and centrifuges after stirring, is obtained acidifying sieving crab shell powder end, acid is washed with deionized
Change sieving crab shell powder, obtain reaction product；
（3）Reaction product and sodium hydroxide solution are mixed and are placed in beaker, continues to keep rotating speed to be mixed, is put into after stirring
Centrifuged in centrifuge, obtain alkalization sieving crab shell powder, then alkalization sieving crab shell powder is washed with deionized, finally put
Enter drying in baking oven, obtain self-control chitin nano fiber；
（4）Weigh 60~80g fish-skins and be put into pulper and blend, obtain fish-skin fragment, by fish-skin fragment, calcium hydroxide and go from
The mixing of sub- water, which is placed in beaker, soaks, and obtains immersion fish-skin, with deionized water cleaning and dipping fish-skin, then will immersion fish-skin and hydrochloric acid
Mixing, which is placed in beaker, soaks, and obtains acidifying fish-skin, with deionized water flush acid fish-skin, until flushing liquor pH is in neutrality, incites somebody to action
Acidifying fish-skin and distilled water mixing after flushing are placed in water-bath and carry glue, and filtering removes filter residue, takes out glue, glue is placed in
Rotated in rotary evaporator, remove moisture removal, obtain self-control gelatin base substrate；
（5）Count in parts by weight, weigh 30~40 parts of self-control gelatin base substrates, 16~20 parts of modified sodium alginates, 12~16 respectively
Part self-control chitin nano fiber and 6~8 parts of silver nitrate solutions mixing are placed in mixer and stir, then add 3~5 parts of shells and gather
Sugar, 2~4 parts of Geniposides, 1~3 part of SODIUM PERCARBONATE and 2~4 parts of ethylenediamines, continue insulation mixing and cure, cooling discharging, i.e.,
Antibacterial heat resistant type gelatin can be made.
Step（1）The mixing time is 16~20min, and the mixing time is 4~6min, stirring the reaction time be
2~4h, mixing reaction time are 1~2h, and the volume ratio of mixed liquor and absolute ethyl alcohol is 1；3, continue that the time is mixed
For 7~9min, washing times are 3~5 times, and drying temperature is 55~65 DEG C, and drying time is 4~6h.
Step（2）The soaking time is 35~45min, and drying temperature is 65~75 DEG C, drying time for 20~
30min, it is 10~12min to grind the time, and the mass ratio for the hydrochloric acid that sieve crab shell powder and mass fraction are 15% is 1：
5, speed of agitator is 300~500r/min, and mixing time is 2~4h, and centrifugal rotational speed is 200~300r/min, during centrifugation
Between be 12~16min, washing times are 3~5 times.
Step（3）The mass ratio for the sodium hydroxide solution that the reaction product and mass fraction is 25% is 1：4, continue
Mixing time is 1~3h, and centrifugal rotational speed is 200~300r/min, and the centrifugation time is 10~12min, drying temperature 60
~70 DEG C, drying time is 2~4h.
Step（4）The time that blends is 5~7min, and the mass ratio of fish-skin fragment, calcium hydroxide and deionized water is
1：2：5, soaking time is 4~6h, and wash number is 2~4 times, soaks the quality of fish-skin and concentration for the hydrochloric acid of 0.06mol/L
Than for 1：4, mixing soaking time is 1~2h, and washing time is 3~5 times, the mass ratio of acidifying fish-skin and distilled water after flushing
For 1：5, glue temperature is put forward as 65~75 DEG C, and it is 2~4h to carry the glue time, and the revolving time is 10~12min.
Step（5）The whipping temp is 55~65 DEG C, and mixing time is 20~30min, continues to stir hardening time
For 1~3h.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention is to make gelatin base substrate by oneself as base material, modified sodium alginate, self-control chitin nano fiber and silver nitrate solution
As reinforcing agent, and it is aided with chitosan, Geniposide and ethylenediamine etc. and antibacterial heat resistant type gelatin is prepared, it is molten first with soda acid
Liquid carries out fish-skin reaction treatment and obtains self-control gelatin base substrate, recycles sodium metaperiodate to be modified sodium alginate, due to sea
Containing two adjacent hydroxyls in one monomeric unit of mosanom, hydroxyl can by sodium periodate oxidation into two aldehyde radicals, and
Oxidized sodium alginate is generated, in preparation process, it is occurred physically or chemically to react with matrix, forms semi-intercrossing network knot
Structure, the heat resistance which is conducive to gelatin are improved, due in sodium alginate containing substantial amounts of-OH and-COO-, in matrix
Contain substantial amounts of-NH2With-COOH, can occur chemically or physically to react between sodium alginate and matrix, and pass through intermolecular interaction
The effects such as power, hydrogen bond and ionic bond are combined, so that the inierpeneirating network structure of molecular level be presented, improve phase therebetween
Interreaction force and compatibility, the heat resistance and mechanical property for being conducive to gelatin are improved；
（2）The present invention from crab shell chitin extraction nanofiber, due to self-control chitin nano fiber can by hydrogen bond with
Chitosan molecule and substrate molecule interaction, when being subject to external force to act on, play the role of transmitting stress, so as to increase
The rotary motion resistance of gelatine polymer segment, improves the crystallinity of gelatin, and the mechanical property for being conducive to gelatin obtains
Improve, be subsequently added into chitosan, wherein chitosan contains free amino group, can be coordinated and be crosslinked with matrix, both are intermolecular can
By interaction of hydrogen bond, to form natural semi-interpenetrating polymer network structure, the heat resistance which is conducive to gelatin obtains
To raising, the in addition in use ,-NH in chitosan molecule3+It is positively charged, adsorb in bacterial cell surface, can also
By penetrating into the intracellular of bacterium, the material that anion is carried in the cell body of bacterium is adsorbed, it is normal to upset bacterial cell
Physiological activity, so as to reach the effect for killing bacterium, improve the antibiotic property of gelatin；
（3）The present invention is modified matrix by silver nitrate solution, is sterilized using catalytic reaction, using silver ion as urging
Change activated centre, the oxygen in hydrone and air activated with matrix, and using generation hydroxyl radical free radical and active oxygen ion come
Destroy bacterial multiplication and realize antibacterial, after thalline loses activity, silver ion and the separate out from thalline, realize durable antibiotic,
The antibiotic property of gelatin is improved again, is eventually adding Geniposide, and Geniposide is crosslinked with matrix, secures alginic acid in the blending process
Sodium, and inierpeneirating network structure is formd, strand is macroscopically shown as since the constraint of crosslinking points can bear larger external force
The increase of interpenetrating network membrane (ipn) tensile strength, further improves the mechanical property of gelatin, is with a wide range of applications.
Embodiment
Weigh 10~12g sodium alginates and pour into 16~20min of mixing in the beaker with 24~32mL absolute ethyl alcohols,
Obtain self-control suspension, then weigh 6~8g sodium metaperiodates pour into the beaker with 32~36mL deionized waters be mixed 4~
6min, obtains self-control solution, and self-control solution is added in above-mentioned self-control suspension, and reaction 2 is mixed at room temperature unglazed
~4h, obtains reaction solution, and 1~2h of reaction is mixed in the ethylene glycol for continuing to add reaction solution volume 3% into reaction solution, obtains
Mixed liquor, is by volume 1；7~9min is mixed in mixed liquor and absolute ethyl alcohol by 3, is filtered and is removed filtrate, uses absolute ethyl alcohol
Wash filter residue 3~5 times, finally the filter residue after washing be put into surface plate, then surface plate is placed in baking oven, in temperature be 55
Dry 4~6h, obtains modified sodium alginate at~65 DEG C；0.4~0.6kg crab shells are weighed to pour into 0.6~0.8L deionized waters
35~45min is soaked, immersion is placed in baking oven, 20~30min is dried at being 65~75 DEG C in temperature, by the crab shell after drying
120 mesh sieves are crossed after grinding 10~12min, sieving crab shell powder is collected, is in mass ratio 1：5 will sieving crab shell powder and matter
The mixed in hydrochloric acid that amount fraction is 15% is placed in beaker, 2~4h is mixed in the case where rotating speed is 300~500r/min, after stirring
It is put into centrifuge, 12~16min is centrifuged under conditions of rotating speed is 200~300r/min, obtains acidifying sieving crab shell
Powder, is washed with deionized acidifying sieving crab shell powder end 3~5 times, obtains reaction product；It is 1 in mass ratio：4 produce reaction
Thing and the sodium hydroxide solution mixing that mass fraction is 25% are placed in beaker, continue to keep rotating speed that 1~3h, stirring is mixed
After be put into centrifuge, rotating speed be 200~300r/min under conditions of centrifuge 10~12min, obtain alkalization sieving crab
Shell powder, then alkalization sieving crab shell powder is washed with deionized, it is finally putting into baking oven, it is dry at being 60~70 DEG C in temperature
2~4h, obtains self-control chitin nano fiber；Weigh 60~80g fish-skins and be put into pulper and blend 5~7min, obtain fish-skin
Fragment, is in mass ratio 1：2：The mixing of fish-skin fragment, calcium hydroxide and deionized water is placed in 4~6h of immersion in beaker by 5, is obtained
Fish-skin is soaked, with deionized water cleaning and dipping fish-skin 2~4 times, then is 1 in mass ratio：Immersion fish-skin and concentration are by 4
The mixed in hydrochloric acid of 0.06mol/L is placed in beaker 1~2h of immersion, obtains acidifying fish-skin, with deionized water flush acid fish-skin 3~
5 times, until flushing liquor pH is in neutrality, it is 1 in mass ratio by the acidifying fish-skin after flushing and distilled water：5 mixing are placed in water-bath
In, 2~4h of glue is carried at being 65~75 DEG C in temperature, filtering removes filter residue, takes out glue, glue is placed in rotary evaporator and is revolved
10~12min is steamed, removes moisture removal, obtains self-control gelatin base substrate；Count in parts by weight, weigh 30~40 parts of self-control gelatin bases respectively
The nitre that body, 16~20 parts of modified sodium alginates, 12~16 parts of self-control chitin nano fibers and 6~8 parts of mass fractions are 15%
Sour silver solution mixing is placed in mixer, stirs 20~30min at being 55~65 DEG C in temperature, then add 3~5 parts of chitosans, 2
~4 parts of Geniposides, 1~3 part of SODIUM PERCARBONATE and 2~4 parts of ethylenediamines, continue insulation be mixed cure 1~3h, cooling discharging,
It can be prepared by antibacterial heat resistant type gelatin.
Example 1
Weigh 10g sodium alginates and pour into the beaker with 24mL absolute ethyl alcohols and 16min is mixed, obtain self-control suspension,
6g sodium metaperiodates are weighed again pour into the beaker with 32mL deionized waters and 4min is mixed, obtain self-control solution, will make by oneself
Solution is added in above-mentioned self-control suspension, and reaction 2h is mixed at room temperature unglazed, obtains reaction solution, continues to reaction solution
Reaction 1h is mixed in the middle ethylene glycol for adding reaction solution volume 3%, obtains mixed liquor, is by volume 1；3 by mixed liquor and
7min is mixed in absolute ethyl alcohol, filters and removes filtrate, washs filter residue 3 times with absolute ethyl alcohol, finally put the filter residue after washing
Enter in surface plate, then surface plate is placed in baking oven, be dry 4h at 55 DEG C in temperature, obtain modified sodium alginate；Weigh
0.4kg crab shells, which are poured into 0.6L deionized waters, soaks 35min, and immersion is placed in baking oven, is dried at being 65 DEG C in temperature
20min, 120 mesh sieves are crossed after the crab shell after drying is ground 10min, are collected sieving crab shell powder, are in mass ratio 1：5 will
Sieving crab shell powder and the mixed in hydrochloric acid that mass fraction is 15% are placed in beaker, are mixed in the case where rotating speed is 300r/min
2h, is put into centrifuge after stirring, and 12min is centrifuged under conditions of rotating speed is 200r/min, obtains acidifying sieving crab shell
Powder, is washed with deionized acidifying sieving crab shell powder end 3 times, obtains reaction product；It is 1 in mass ratio：4 by reaction product and
The sodium hydroxide solution mixing that mass fraction is 25% is placed in beaker, is continued to keep rotating speed that 1h is mixed, is put into after stirring
In centrifuge, rotating speed be 200r/min under conditions of centrifuge 10min, obtain alkalization sieving crab shell powder, then spend from
Sub- water washing alkalization sieving crab shell powder, is finally putting into baking oven, and dry 2h at being 60 DEG C in temperature, obtains self-control chitin and receive
Rice fiber；Weigh 60g fish-skins and be put into pulper and blend 5min, obtain fish-skin fragment, be in mass ratio 1：2：5 is broken by fish-skin
Piece, calcium hydroxide and deionized water mixing are placed in beaker and soak 4h, immersion fish-skin are obtained, with deionized water cleaning and dipping fish-skin
2 times, then be 1 in mass ratio：4 will soak the mixed in hydrochloric acid that fish-skin and concentration are 0.06mol/L and be placed in beaker and soak 1h, obtain
Fish-skin is acidified, with deionized water flush acid fish-skin 3 times, until flushing liquor pH is in neutrality, by the acidifying fish-skin after flushing and steaming
Distilled water is 1 in mass ratio：5 mixing are placed in water-bath, and glue 2h is carried at being 65 DEG C in temperature, and filtering removes filter residue, takes out glue,
Glue is placed in rotary evaporator and rotates 10min, removes moisture removal, obtains self-control gelatin base substrate；Count, claim respectively in parts by weight
It is 15% to take 30 parts of self-control gelatin base substrates, 16 parts of modified sodium alginates, 12 parts of self-control chitin nano fibers and 6 parts of mass fractions
Silver nitrate solution mixing be placed in mixer, stir 20min at being 55 DEG C in temperature, then add 3 parts of chitosans, 2 parts of capital Buddhist nuns
Flat, 1 part of SODIUM PERCARBONATE and 2 parts of ethylenediamines, continue insulation and curing 1h, cooling discharging are mixed, you can antibacterial heat resistant type is made
Gelatin.
Example 2
Weigh 11g sodium alginates and pour into the beaker with 28mL absolute ethyl alcohols and 18min is mixed, obtain self-control suspension,
7g sodium metaperiodates are weighed again pour into the beaker with 34mL deionized waters and 5min is mixed, obtain self-control solution, will make by oneself
Solution is added in above-mentioned self-control suspension, and reaction 3h is mixed at room temperature unglazed, obtains reaction solution, continues to reaction solution
Reaction 1.5h is mixed in the middle ethylene glycol for adding reaction solution volume 3%, obtains mixed liquor, is by volume 1；3 by mixed liquor
8min is mixed with absolute ethyl alcohol, filters and removes filtrate, filter residue is washed 4 times with absolute ethyl alcohol, finally by the filter residue after washing
It is put into surface plate, then surface plate is placed in baking oven, is dry 5h at 60 DEG C in temperature, obtains modified sodium alginate；Weigh
0.5kg crab shells, which are poured into 0.7L deionized waters, soaks 40min, and immersion is placed in baking oven, is dried at being 70 DEG C in temperature
25min, 120 mesh sieves are crossed after the crab shell after drying is ground 11min, are collected sieving crab shell powder, are in mass ratio 1：5 will
Sieving crab shell powder and the mixed in hydrochloric acid that mass fraction is 15% are placed in beaker, are mixed in the case where rotating speed is 400r/min
3h, is put into centrifuge after stirring, and 14min is centrifuged under conditions of rotating speed is 250r/min, obtains acidifying sieving crab shell
Powder, is washed with deionized acidifying sieving crab shell powder end 4 times, obtains reaction product；It is 1 in mass ratio：4 by reaction product and
The sodium hydroxide solution mixing that mass fraction is 25% is placed in beaker, is continued to keep rotating speed that 2h is mixed, is put into after stirring
In centrifuge, rotating speed be 250r/min under conditions of centrifuge 11min, obtain alkalization sieving crab shell powder, then spend from
Sub- water washing alkalization sieving crab shell powder, is finally putting into baking oven, and dry 3h at being 65 DEG C in temperature, obtains self-control chitin and receive
Rice fiber；Weigh 70g fish-skins and be put into pulper and blend 6min, obtain fish-skin fragment, be in mass ratio 1：2：5 is broken by fish-skin
Piece, calcium hydroxide and deionized water mixing are placed in beaker and soak 5h, immersion fish-skin are obtained, with deionized water cleaning and dipping fish-skin
3 times, then be 1 in mass ratio：4 will soak the mixed in hydrochloric acid that fish-skin and concentration are 0.06mol/L and be placed in beaker and soak 1.5h, obtain
To acidifying fish-skin, with deionized water flush acid fish-skin 4 times, until flushing liquor pH is in neutrality, by the acidifying fish-skin after flushing and
Distilled water is 1 in mass ratio：5 mixing are placed in water-bath, carry glue 3h at being 70 DEG C in temperature, filtering removes filter residue, takes out glue
Liquid, glue is placed in rotary evaporator and rotates 11min, removes moisture removal, obtains self-control gelatin base substrate；Count in parts by weight, point
Nickname takes 35 parts to make gelatin base substrates, 18 parts of modified sodium alginates, 14 parts of self-control chitin nano fibers and 7 parts of mass fractions by oneself
15% silver nitrate solution mixing be placed in mixer, temperature be 60 DEG C at stir 25min, then add 4 parts of chitosans, 3 parts
Geniposide, 2 parts of SODIUM PERCARBONATEs and 3 parts of ethylenediamines, continue insulation and curing 2h, cooling discharging are mixed, you can it is resistance to that antibacterial is made
Heat type gelatin.
Example 3
Weigh 12g sodium alginates and pour into the beaker with 32mL absolute ethyl alcohols and 20min is mixed, obtain self-control suspension,
8g sodium metaperiodates are weighed again pour into the beaker with 36mL deionized waters and 6min is mixed, obtain self-control solution, will make by oneself
Solution is added in above-mentioned self-control suspension, and reaction 4h is mixed at room temperature unglazed, obtains reaction solution, continues to reaction solution
Reaction 2h is mixed in the middle ethylene glycol for adding reaction solution volume 3%, obtains mixed liquor, is by volume 1；3 by mixed liquor and
9min is mixed in absolute ethyl alcohol, filters and removes filtrate, washs filter residue 5 times with absolute ethyl alcohol, finally put the filter residue after washing
Enter in surface plate, then surface plate is placed in baking oven, be dry 6h at 65 DEG C in temperature, obtain modified sodium alginate；Weigh
0.6kg crab shells, which are poured into 0.8L deionized waters, soaks 45min, and immersion is placed in baking oven, is dried at being 75 DEG C in temperature
30min, 120 mesh sieves are crossed after the crab shell after drying is ground 12min, are collected sieving crab shell powder, are in mass ratio 1：5 will
Sieving crab shell powder and the mixed in hydrochloric acid that mass fraction is 15% are placed in beaker, are mixed in the case where rotating speed is 500r/min
4h, is put into centrifuge after stirring, and 16min is centrifuged under conditions of rotating speed is 300r/min, obtains acidifying sieving crab shell
Powder, is washed with deionized acidifying sieving crab shell powder end 5 times, obtains reaction product；It is 1 in mass ratio：4 by reaction product and
The sodium hydroxide solution mixing that mass fraction is 25% is placed in beaker, is continued to keep rotating speed that 3h is mixed, is put into after stirring
In centrifuge, rotating speed be 300r/min under conditions of centrifuge 12min, obtain alkalization sieving crab shell powder, then spend from
Sub- water washing alkalization sieving crab shell powder, is finally putting into baking oven, and dry 4h at being 70 DEG C in temperature, obtains self-control chitin and receive
Rice fiber；Weigh 80g fish-skins and be put into pulper and blend 7min, obtain fish-skin fragment, be in mass ratio 1：2：5 is broken by fish-skin
Piece, calcium hydroxide and deionized water mixing are placed in beaker and soak 6h, immersion fish-skin are obtained, with deionized water cleaning and dipping fish-skin
4 times, then be 1 in mass ratio：4 will soak the mixed in hydrochloric acid that fish-skin and concentration are 0.06mol/L and be placed in beaker and soak 2h, obtain
Fish-skin is acidified, with deionized water flush acid fish-skin 5 times, until flushing liquor pH is in neutrality, by the acidifying fish-skin after flushing and steaming
Distilled water is 1 in mass ratio：5 mixing are placed in water-bath, and glue 4h is carried at being 75 DEG C in temperature, and filtering removes filter residue, takes out glue,
Glue is placed in rotary evaporator and rotates 12min, removes moisture removal, obtains self-control gelatin base substrate；Count, claim respectively in parts by weight
It is 15% to take 40 parts of self-control gelatin base substrates, 20 parts of modified sodium alginates, 16 parts of self-control chitin nano fibers and 8 parts of mass fractions
Silver nitrate solution mixing be placed in mixer, stir 30min at being 65 DEG C in temperature, then add 5 parts of chitosans, 4 parts of capital Buddhist nuns
Flat, 3 parts of SODIUM PERCARBONATEs and 4 parts of ethylenediamines, continue insulation and curing 3h, cooling discharging are mixed, you can antibacterial heat resistant type is made
Gelatin.
Comparative example
With the gelatin of company of Jinan City production as a comparison case
Gelatin in antibacterial heat resistant type gelatin produced by the present invention and comparative example is detected, testing result is as shown in table 1：
1st, physical and mechanical property test
Example 1~3 and comparative example product prepared by the 7.5g present invention are weighed, is dissolved separately in 105mL distilled water, then pour into jelly
In power bottle, bottleneck is clogged with plug, is put into water-bath and heats, and be placed on 15min at room temperature, obtain 6.67% glue sample.It will freeze
Power bottle is put into constant temperature（Kept for 10 DEG C）In cold bath, 16~18h is placed.Adjustment upper contact and the interval of lower contact are equal to 4mm, use
The plunger press-in frozen glue surface of a diameter of 12.7mm, record is allowed to produce the required weight of depression of 4mm depths, is glue sample
Bo Lumu power.
2nd, heat stability testing
Example 1~3 and comparative example product prepared by the present invention, is respectively placed in 65 DEG C, 75 DEG C and 85 DEG C of water bath with thermostatic control and adds
Hot 30min, makes its inactivation, rear stored refrigerated 24h, makes its renaturation.At room temperature by the sample after 0.5g renaturation, concentration 25mol/
The 4- nitrobenzophenone palmitate 1mL and concentration of mL is 10mol/mL, and the phosphate buffer solution 2mL of pH=7.50 is quickly mixed
After conjunction, the absorbance change by UV spectrophotometer measuring reaction solution at 400nm immediately, by the absorbance with without adding
The gelatin of heat is compared through the absorbance obtained by same test under the same reaction conditions, obtains relative activity.
Table 1
From the data in table 1, it can be seen that antibacterial heat resistant type gelatin produced by the present invention, mechanical property is good, biocidal property is strong, heat endurance is good,
It is substantially better than comparative example product.Therefore, there is wide prospect of the application.
Claims (6)
1. a kind of preparation method of antibacterial heat resistant type gelatin, it is characterised in that specifically preparation process is：
（1）Weigh 10~12g sodium alginates and pour into the beaker with 24~32mL absolute ethyl alcohols and be mixed, it is outstanding to obtain self-control
Supernatant liquid, then weigh 6~8g sodium metaperiodates and pour into the beaker with 32~36mL deionized waters and be mixed, obtain making by oneself molten
Liquid, self-control solution is added in above-mentioned self-control suspension, and reaction is mixed at room temperature unglazed, obtains reaction solution, continues
Reaction is mixed in the ethylene glycol that reaction solution volume 3% is added into reaction solution, mixed liquor is obtained, by mixed liquor and absolute ethyl alcohol
It is mixed, filters and remove filtrate, wash filter residue with absolute ethyl alcohol, finally the filter residue after washing is put into surface plate, by table
Face ware is placed in drying in baking oven, obtains modified sodium alginate；
（2）Weigh 0.4~0.6kg crab shells and pour into 0.6~0.8L deionized waters and soak, immersion, which is placed in baking oven, dries, and dries
120 mesh sieves are crossed after crab shell is ground after dry, collect sieving crab shell powder, sieving crab shell powder and mixed in hydrochloric acid are placed in burning
It is mixed in cup, is put into centrifuge and centrifuges after stirring, is obtained acidifying sieving crab shell powder end, acid is washed with deionized
Change sieving crab shell powder, obtain reaction product；
（3）Reaction product and sodium hydroxide solution are mixed and are placed in beaker, continues to keep rotating speed to be mixed, is put into after stirring
Centrifuged in centrifuge, obtain alkalization sieving crab shell powder, then alkalization sieving crab shell powder is washed with deionized, finally put
Enter drying in baking oven, obtain self-control chitin nano fiber；
（4）Weigh 60~80g fish-skins and be put into pulper and blend, obtain fish-skin fragment, by fish-skin fragment, calcium hydroxide and go from
The mixing of sub- water, which is placed in beaker, soaks, and obtains immersion fish-skin, with deionized water cleaning and dipping fish-skin, then will immersion fish-skin and hydrochloric acid
Mixing, which is placed in beaker, soaks, and obtains acidifying fish-skin, with deionized water flush acid fish-skin, until flushing liquor pH is in neutrality, incites somebody to action
Acidifying fish-skin and distilled water mixing after flushing are placed in water-bath and carry glue, and filtering removes filter residue, takes out glue, glue is placed in
Rotated in rotary evaporator, remove moisture removal, obtain self-control gelatin base substrate；
（5）Count in parts by weight, weigh 30~40 parts of self-control gelatin base substrates, 16~20 parts of modified sodium alginates, 12~16 respectively
Part self-control chitin nano fiber and 6~8 parts of silver nitrate solutions mixing are placed in mixer and stir, then add 3~5 parts of shells and gather
Sugar, 2~4 parts of Geniposides, 1~3 part of SODIUM PERCARBONATE and 2~4 parts of ethylenediamines, continue insulation mixing and cure, cooling discharging, i.e.,
Antibacterial heat resistant type gelatin can be made.
A kind of 2. preparation method of antibacterial heat resistant type gelatin according to claim 1, it is characterised in that：Step（1）It is described
Mixing time be 16~20min, the mixing time is 4~6min, and the stirring reaction time is 2~4h, be mixed reaction
Time is 1~2h, and the volume ratio of mixed liquor and absolute ethyl alcohol is 1；3, it is 7~9min to continue to be mixed the time, washing times
For 3~5 times, drying temperature is 55~65 DEG C, and drying time is 4~6h.
A kind of 3. preparation method of antibacterial heat resistant type gelatin according to claim 1, it is characterised in that：Step（2）It is described
Soaking time be 35~45min, drying temperature is 65~75 DEG C, and drying time be 20~30min, and it is 10 to grind the time
~12min, the mass ratio for the hydrochloric acid that sieve crab shell powder and mass fraction are 15% is 1：5, speed of agitator is 300~500r/
Min, mixing time are 2~4h, and centrifugal rotational speed is 200~300r/min, and the centrifugation time is 12~16min, washing times
For 3~5 times.
A kind of 4. preparation method of antibacterial heat resistant type gelatin according to claim 1, it is characterised in that：Step（3）It is described
Reaction product and mass fraction be 25% the mass ratio of sodium hydroxide solution be 1：4, continuation mixing time is 1~3h, from
Heart rotating speed is 200~300r/min, and the centrifugation time is 10~12min, and drying temperature is 60~70 DEG C, drying time 2
~4h.
A kind of 5. preparation method of antibacterial heat resistant type gelatin according to claim 1, it is characterised in that：Step（4）It is described
The time that blends be 5~7min, the mass ratio of fish-skin fragment, calcium hydroxide and deionized water is 1：2：5, soaking time for 4~
6h, wash number are 2~4 times, and the mass ratio for soaking the hydrochloric acid that fish-skin and concentration are 0.06mol/L is 1：4, mix soaking time
For 1~2h, washing time is 3~5 times, and the mass ratio of acidifying fish-skin and distilled water after flushing is 1：5, carry glue temperature for 65~
75 DEG C, it is 2~4h to carry the glue time, and the revolving time is 10~12min.
A kind of 6. preparation method of antibacterial heat resistant type gelatin according to claim 1, it is characterised in that：Step（5）It is described
Whipping temp be 55~65 DEG C, mixing time be 20~30min, continue stirring hardening time be 1~3h.
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| CN111529209A (en) * | 2020-05-07 | 2020-08-14 | 关怡 | Medical sanitary non-woven fabric |
| CN115477506A (en) * | 2022-07-25 | 2022-12-16 | 马鞍山市申锐节能新材料有限公司 | Thermal insulation mortar with high crack resistance and preparation method thereof |
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