CN108193311A - A kind of preparation method of fibroin albumen sodium alginate composite fiber - Google Patents
A kind of preparation method of fibroin albumen sodium alginate composite fiber Download PDFInfo
- Publication number
- CN108193311A CN108193311A CN201711278052.5A CN201711278052A CN108193311A CN 108193311 A CN108193311 A CN 108193311A CN 201711278052 A CN201711278052 A CN 201711278052A CN 108193311 A CN108193311 A CN 108193311A
- Authority
- CN
- China
- Prior art keywords
- sodium alginate
- fibroin albumen
- composite fiber
- carbomer
- constant temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/43504—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates
- C07K14/43563—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from insects
- C07K14/43586—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from insects from silkworms
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P21/00—Preparation of peptides or proteins
- C12P21/06—Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
Abstract
The invention discloses a kind of preparation methods of fibroin albumen sodium alginate composite fiber, belong to natural high molecular composite material preparing technical field.Stirring and dissolving after the present invention first mixes fibroin albumen and water, it is centrifuged after dialysis, silk fibroin protein solution must be pre-processed, pH is adjusted after elastoser and pretreatment silk fibroin protein solution are mixed, constant temperature stirring enzymolysis, obtain enzymolysis liquid, ultrasonic disperse after then mixing phosphatide and enzymolysis liquid, add sodium alginate, plants essential oil and monosaccharide, constant temperature is stirred to react, obtain reaction solution, after reaction solution and carbomer are mixed again, constant temperature is stirred to react, obtain spinning solution, the spinning after vacuum defoamation again, and through washing, drawing-off, curling and drying, obtain fibroin albumen sodium alginate composite fiber.Gained fibroin albumen sodium alginate composite fiber of the invention has good mechanical property.
Description
Technical field
The invention discloses a kind of preparation methods of fibroin albumen sodium alginate composite fiber, and it is compound to belong to natural polymer
Technical field of material.
Background technology
Sodium alginate（SA）It is a kind of macromolecule polysaccharide extracted from brown alga, is ancient by beta-D-mannuronic acid and α-L-
A kind of linear polymer that sieve uronic acid is formed by 1-4 glucosides key connections due to its good biocompatibility, can naturally drop
The performances such as solution property and high fire-retardance, have a wide range of applications in fields such as biologic medical, food, sewage disposal and weavings.Alginic acid
Sodium ion and divalent metal in sodium（Mg2+Except）Fast ion exchange occurs to react, the G in sodium alginate structure is mono-
Member is combined even closer with divalent metal, forms special " eggshell structure ", last G units are accumulated to form hydrogel
Be precipitated, sodium alginate fiber be is prepared according to this principle by the method for wet spinning it is molding, but due to sodium alginate divide
Subchain section is in rigidity, and strand, which always closely overlaps, cannot form effective chain entanglement, thus sodium alginate is fine
Dimension lacks intensity and elasticity, mechanical property are poor.In recent years, research shows that sodium alginate gathers with krill albumen, cellulose and shell
The mechanical property of composite material can be improved after the natural macromolecular materials such as sugar are compound.
Fibroin albumen（SF）It is the main component of silk cocoon, is made of 18 kinds of amino acid, the silk peptide tool in fibroin albumen
There are remarkable skin care, strong skin, hair care cosmetology function, and with good biocompatibility.Due to the amino in fibroin albumen
Acid has a large amount of amino, hydroxyl and amide group, contains a large amount of hydroxyl group in sodium alginate, fibroin albumen and seaweed
Hydrogen bond action between sour sodium complicated utilization hydroxyl-hydroxyl, hydroxy-amide base, amino-carbonyl improves fibroin albumen and alginic acid
Active force between sodium molecule improves the mechanical property of composite fibre, in order to further improve the mechanical property of composite fibre, drawing
The fibroin albumen progress entered is chemical crosslinking modified, and generating a kind of tridimensional network increases the non-deformability of composite fibre, mesh
The crosslinking agent of preceding crosslinking fibroin albumen mainly has Geniposide, carbodiimides, ethylene glycol diglycidylether and glutaraldehyde etc., main
If some small molecule crosslinking agents, the polyethyleneglycol diglycidylether of selection（PEGDE, Mn ≈ 400）It is a kind of low molecular weight
Crosslinking agent, structure is similar to ethylene glycol diglycidylether, has the characteristics that flexibility is good, viscosity is low.PEGDE contains greatly
Ring-opening reaction, the old reaction for having studied ethylene glycol diglycidylether crosslinking fibroin albumen, ethylene glycol two easily occur for the ehter bond of amount
After the epoxy group open loop at glycidol ether both ends with the key reaction site of fibroin albumen tyrosine benzene hydroxyl, lysine
Amino and histidine imidazole ring imino group on, reaction generates a kind of tridimensional network.Therefore it also needs to carry out it
Research, the mechanical property to enhance fibroin albumen sodium alginate composite fiber are provided according to reference.
Invention content
The present invention solves the technical problem of：For traditional fibroin albumen sodium alginate composite fiber mechanical property not
The problem of good, provides a kind of preparation method of fibroin albumen sodium alginate composite fiber
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）It is 1 in mass ratio by fibroin albumen and water：40~1：50 mix, and after constant temperature stirring and dissolving, are transferred to bag filter, dialysis 4
~6 days, then be centrifuged, obtain pretreatment silk fibroin protein solution；
（2）It is 1 in mass ratio by elastoser and pretreatment silk fibroin protein solution：500~1：After 600 mixing, pH is adjusted, then
It stirs and digests through constant temperature, obtain enzymolysis liquid；
（3）It counts in parts by weight, takes 8~10 parts of phosphatide, 4~8 parts of sodium alginates, 1~4 part of monosaccharide, 2~4 parts of plant essences successively
Oil, 100~120 parts of enzymolysis liquids, ultrasonic disperse after first mixing phosphatide and enzymolysis liquid, add sodium alginate, plants essential oil and
Monosaccharide, constant temperature are stirred to react, and obtain reaction solution；
（4）It is 1 in mass ratio by reaction solution and carbomer liquid：1~3：After 1 mixing, constant temperature is stirred to react, and obtains spinning solution, then pass through
Spinning after vacuum defoamation, and through washing, drawing-off, curling and drying, obtain fibroin albumen sodium alginate composite fiber.
Step（1）The bag filter specification is：Molecular cut off is 10~12kDa.
Step（2）The pH is 7.6~7.8.
Step（3）The phosphatide is any one in soybean lecithin or egg lecithin.
Step（3）The monosaccharide is any one in glucose, fructose or galactolipin.
Step（3）The plants essential oil is any one in Lavender, tea tree ethereal oil or camellia flower essential oil.
Step（4）The carbomer liquid configuration process is：It is 1 in mass ratio by carbomer and water：30~1：After 35 mixing,
Standing swelling 20~for 24 hours, then heated stirring and dissolving, obtain carbomer liquid；The carbomer for Acritamer 940, Carbopol 941 or
Any one in carbomer 937.
The beneficial effects of the invention are as follows：
（1）Technical solution of the present invention digests fibroin albumen first with elastoser, free amino group in raising system
Quantity, recycle the carbonyl in free amino group and monosaccharide that condensation reaction occurs, ultimately form stable cross-linked polymer, so as to
The glucide in fibroin albumen and system is made to form stable cross-linked network system, so as to which product tensile strength be made to obtain effectively
It is promoted, and the addition of phosphatide, it is because fibroin albumen is after elastin laminin enzyme hydrolysis, partial hydrolysate is easily reunited,
And make active group and glucide that can not come into full contact with, and phosphatide is because with more negative electrical charge group in molecular structure, it can
Make fibroin albumen hydrolysate mutually exclusive when carrying same sex charge, therefore be stably dispersed in system, so as to make crosslinking
Network system consistency is effectively promoted, and the mechanical properties such as product tensile strength is made further to be promoted, and phosphatide is also
Surfactant can be used as, is conducive to improve permeance property of the plants essential oil to product system, and after plants essential oil use, it can
The position of part functional group in cross-linked network molecular structure is occupied, the oscillation intensity of covalent bond in molecular structure is reduced, makes mechanics
Performance is positively maintained, and hydrophilic radical is reduced in fiber product, and fibrous inside moisture content reduces, so as to effectively avoid fiber
The problem of leading to mechanical properties decrease due to during storage and use because water absorption and swelling；
（2）Technical solution of the present invention is by adding carbomer, containing more acid groups in carbomer molecular structure, can in system
Dehydrating condensation occurs for the free amino group that hydrolysis generates, and amido bond is formed, so as to make carbomer molecular structure and cross-linked network structure
Chemical bonding is generated, in addition, after part carboxyl is ionized in carbomer molecular structure, due to the mutually exclusive work of negative electrical charge
With stretching strand disperse, in great swelling state, and with stickiness, so as to the object with carrying saccharide residue in system
Matter forms Hydrogenbond, stronger mucous gels network is generated, so as to which the mechanical properties such as system tensile strength be made to obtain further
It is promoted.
Specific embodiment
It is 1 in mass ratio by carbomer and water：30~1：35 mixing after, under room temperature stand swelling 20~for 24 hours, then
It it is 65~75 DEG C in temperature, under the conditions of rotating speed is 200~300r/min, heating stirring dissolving obtains carbomer liquid；By fibroin albumen
It is 1 in mass ratio with water：40~1：50 mixing are poured into beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, in
Temperature is 70~80 DEG C, and under the conditions of rotating speed is 300~500r/min, after 1~2h of constant temperature stirring and dissolving, material in beaker is poured into
Molecular cut off is in the bag filter of 10~12kDa, and bag filter is placed in deionized water, is dialysed 4~6 days, during dialysis
A water is changed every 3~5h, after rotating speed to centrifuge 5~10min under the conditions of 8000~12000r/min to the end of dialysis,
Supernatant liquor is collected, obtains pretreatment silk fibroin protein solution；It is in mass ratio by elastoser and pretreatment silk fibroin protein solution
1：500~1：Three-necked flask is poured into 600 mixing, and adjusts material pH to 7.6~7.8 in three-necked flask with triethanolamine solution,
Three-necked flask immigration digital display is tested the speed constant temperature blender with magnetic force again, is 40~45 DEG C in temperature, rotating speed is 400~600r/min items
Under part, after 3~5h of constant temperature stirring enzymolysis, 90~95 DEG C are warming up to, 10~15min of enzyme deactivation is kept the temperature, after naturally cool to room temperature, obtains
Enzymolysis liquid；It counts in parts by weight, takes 8~10 parts of phosphatide, 4~8 parts of sodium alginates, 1~4 part of monosaccharide, 2~4 parts of plant essences successively
Oil, 100~120 parts of enzymolysis liquids are 45~55kHz in supersonic frequency, temperature is 45~55 after first mixing phosphatide and enzymolysis liquid
45~60min of ultrasonic disperse under the conditions of DEG C, obtains dispersion liquid, and dispersion liquid is moved into reaction kettle, then to filling the anti-of dispersion liquid
It answers and sodium alginate, plants essential oil and monosaccharide is sequentially added in kettle, be 95~100 DEG C in temperature, rotating speed is 600~800r/min items
Under part, constant temperature is stirred to react 2~4h, obtains reaction solution；It is again 1 in mass ratio by gained reaction solution and carbomer liquid：1~3：1 is mixed
It is 65~80 DEG C in temperature after conjunction, under the conditions of rotating speed is 500~600r/min, constant temperature is stirred to react 2~4h, obtains spinning solution, and
By gained spinning solution 10~20min of vacuum defoamation, then by the spinning solution after deaeration after centrifugal spinning, wash 3~5 times, then pass through
After drawing-off, curling, dry to constant weight, discharged to get the compound fibre of fibroin albumen sodium alginate under the conditions of being 80~90 DEG C in temperature
Dimension.The phosphatide is any one in soybean lecithin or egg lecithin.The monosaccharide is glucose, fructose or galactolipin
In any one.The plants essential oil is any one in Lavender, tea tree ethereal oil or camellia flower essential oil.The card
Wave nurse is any one in Acritamer 940, Carbopol 941 or carbomer 937.
Example 1
It is 1 in mass ratio by carbomer and water：It is 75 DEG C then at temperature in standing swelling for 24 hours under room temperature after 35 mixing,
Under the conditions of rotating speed is 300r/min, heating stirring dissolving obtains carbomer liquid；It is 1 in mass ratio by fibroin albumen and water：50 mixing
It pours into beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, be 80 DEG C in temperature, rotating speed is 500r/min conditions
Under, after constant temperature stirring and dissolving 2h, material in beaker is poured into the bag filter that molecular cut off is 12kDa, and bag filter is put
In deionized water, dialyse 6 days, change a water every 5h during dialysis, when dialysis terminate after rotating speed be 12000r/min items
10min is centrifuged under part, supernatant liquor is collected, obtains pretreatment silk fibroin protein solution；By elastoser and pretreatment fibroin
Protein solution is 1 in mass ratio：Three-necked flask is poured into 600 mixing, and adjusts material pH in three-necked flask with triethanolamine solution
It tests the speed constant temperature blender with magnetic force to 7.8, then by three-necked flask immigration digital display, is 45 DEG C in temperature, rotating speed is 600r/min conditions
Under, after constant temperature stirring enzymolysis 5h, 95 DEG C are warming up to, enzyme deactivation 15min is kept the temperature, after naturally cool to room temperature, obtains enzymolysis liquid；By weight
Number meter, takes 10 parts of phosphatide successively, 8 parts of sodium alginates, 4 parts of monosaccharide, 4 parts of plants essential oils, 120 parts of enzymolysis liquids, first by phosphatide and
It is 55kHz in supersonic frequency after enzymolysis liquid mixing, temperature is ultrasonic disperse 60min under the conditions of 55 DEG C, obtains dispersion liquid, and will divide
Dispersion liquid is moved into reaction kettle, then sodium alginate, plants essential oil and monosaccharide, Yu Wen are sequentially added into the reaction kettle for fill dispersion liquid
It is 100 DEG C to spend, and under the conditions of rotating speed is 800r/min, constant temperature is stirred to react 4h, obtains reaction solution；Again by gained reaction solution and carbomer
Liquid is 3 in mass ratio：It it is 80 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature is stirred to react 4h, obtains spinning after 1 mixing
Liquid, and by gained spinning solution vacuum defoamation 20min, then by the spinning solution after deaeration after centrifugal spinning, wash 5 times, then through leading
After stretching, crimping, dry to constant weight, discharged to get fibroin albumen sodium alginate composite fiber under the conditions of being 90 DEG C in temperature.It is described
Phosphatide is soybean lecithin.The monosaccharide is glucose.The plants essential oil is Lavender.The carbomer is carbomer
940。
Example 2
It is 1 in mass ratio by carbomer and water：It is 75 DEG C then at temperature in standing swelling for 24 hours under room temperature after 35 mixing,
Under the conditions of rotating speed is 300r/min, heating stirring dissolving obtains carbomer liquid；It is 1 in mass ratio by fibroin albumen and water：50 mixing
It pours into beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, be 80 DEG C in temperature, rotating speed is 500r/min conditions
Under, after constant temperature stirring and dissolving 2h, material in beaker is poured into the bag filter that molecular cut off is 12kDa, and bag filter is put
In deionized water, dialyse 6 days, change a water every 5h during dialysis, when dialysis terminate after rotating speed be 12000r/min items
10min is centrifuged under part, supernatant liquor is collected, obtains pretreatment silk fibroin protein solution；It counts in parts by weight, takes 10 parts of phosphorus successively
Fat, 8 parts of sodium alginates, 4 parts of monosaccharide, 4 parts of plants essential oils, 120 parts of pretreatment silk fibroin protein solutions, first by phosphatide and pretreatment silk
It is 55kHz in supersonic frequency after the mixing of fibroin solution, temperature is ultrasonic disperse 60min under the conditions of 55 DEG C, obtains dispersion liquid, and
Dispersion liquid is moved into reaction kettle, then sodium alginate, plants essential oil and monosaccharide are sequentially added into the reaction kettle for fill dispersion liquid,
It it is 100 DEG C in temperature, under the conditions of rotating speed is 800r/min, constant temperature is stirred to react 4h, obtains reaction solution；Again by gained reaction solution and card
Wave nurse liquid is 3 in mass ratio：It it is 80 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature is stirred to react 4h, obtains after 1 mixing
Spinning solution, and by gained spinning solution vacuum defoamation 20min, then by the spinning solution after deaeration after centrifugal spinning, wash 5 times, then
After drawing-off, curling, dry to constant weight, discharged to get fibroin albumen sodium alginate composite fiber under the conditions of being 90 DEG C in temperature.
The phosphatide is soybean lecithin.The monosaccharide is glucose.The plants essential oil is Lavender.The carbomer is card
Wave nurse 940.
Example 3
It is 1 in mass ratio by carbomer and water：It is 75 DEG C then at temperature in standing swelling for 24 hours under room temperature after 35 mixing,
Under the conditions of rotating speed is 300r/min, heating stirring dissolving obtains carbomer liquid；It is 1 in mass ratio by fibroin albumen and water：50 mixing
It pours into beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, be 80 DEG C in temperature, rotating speed is 500r/min conditions
Under, after constant temperature stirring and dissolving 2h, material in beaker is poured into the bag filter that molecular cut off is 12kDa, and bag filter is put
In deionized water, dialyse 6 days, change a water every 5h during dialysis, when dialysis terminate after rotating speed be 12000r/min items
10min is centrifuged under part, supernatant liquor is collected, obtains pretreatment silk fibroin protein solution；By elastoser and pretreatment fibroin
Protein solution is 1 in mass ratio：Three-necked flask is poured into 600 mixing, and adjusts material pH in three-necked flask with triethanolamine solution
It tests the speed constant temperature blender with magnetic force to 7.8, then by three-necked flask immigration digital display, is 45 DEG C in temperature, rotating speed is 600r/min conditions
Under, after constant temperature stirring enzymolysis 5h, 95 DEG C are warming up to, enzyme deactivation 15min is kept the temperature, after naturally cool to room temperature, obtains enzymolysis liquid；By weight
Number meter takes 8 parts of sodium alginates successively, and 4 parts of monosaccharide, 4 parts of plants essential oils, 120 parts of enzymolysis liquids will be with enzymolysis liquid in supersonic frequency
For 55kHz, temperature is ultrasonic disperse 60min under the conditions of 55 DEG C, obtains dispersion liquid, and dispersion liquid is moved into reaction kettle, then to Sheng
Sodium alginate, plants essential oil and monosaccharide are sequentially added in the reaction kettle for having dispersion liquid, in temperature be 100 DEG C, rotating speed 800r/
Under the conditions of min, constant temperature is stirred to react 4h, obtains reaction solution；It is again 3 in mass ratio by gained reaction solution and carbomer liquid：1 mixing
Afterwards, it is 80 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature is stirred to react 4h, obtains spinning solution, and gained spinning solution is true
Empty deaeration 20min, then by the spinning solution after deaeration after centrifugal spinning is washed 5 times, then after drawing-off, curling, in temperature be 90
It dries to constant weight, is discharged to get fibroin albumen sodium alginate composite fiber under the conditions of DEG C.The monosaccharide is glucose.The plant
Object essential oil is Lavender.The carbomer is Acritamer 940.
Example 4
It is 1 in mass ratio by carbomer and water：It is 75 DEG C then at temperature in standing swelling for 24 hours under room temperature after 35 mixing,
Under the conditions of rotating speed is 300r/min, heating stirring dissolving obtains carbomer liquid；It is 1 in mass ratio by fibroin albumen and water：50 mixing
It pours into beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, be 80 DEG C in temperature, rotating speed is 500r/min conditions
Under, after constant temperature stirring and dissolving 2h, material in beaker is poured into the bag filter that molecular cut off is 12kDa, and bag filter is put
In deionized water, dialyse 6 days, change a water every 5h during dialysis, when dialysis terminate after rotating speed be 12000r/min items
10min is centrifuged under part, supernatant liquor is collected, obtains pretreatment silk fibroin protein solution；By elastoser and pretreatment fibroin
Protein solution is 1 in mass ratio：Three-necked flask is poured into 600 mixing, and adjusts material pH in three-necked flask with triethanolamine solution
It tests the speed constant temperature blender with magnetic force to 7.8, then by three-necked flask immigration digital display, is 45 DEG C in temperature, rotating speed is 600r/min conditions
Under, after constant temperature stirring enzymolysis 5h, 95 DEG C are warming up to, enzyme deactivation 15min is kept the temperature, after naturally cool to room temperature, obtains enzymolysis liquid；By weight
Number meter, takes 10 parts of phosphatide successively, 8 parts of sodium alginates, 4 parts of monosaccharide, 120 parts of enzymolysis liquids, after first phosphatide and enzymolysis liquid are mixed,
It is 55kHz in supersonic frequency, temperature is ultrasonic disperse 60min under the conditions of 55 DEG C, obtains dispersion liquid, and dispersion liquid is moved into reaction kettle
In, then sodium alginate and monosaccharide are sequentially added into the reaction kettle for fill dispersion liquid, in temperature be 100 DEG C, rotating speed 800r/
Under the conditions of min, constant temperature is stirred to react 4h, obtains reaction solution；It is again 3 in mass ratio by gained reaction solution and carbomer liquid：1 mixing
Afterwards, it is 80 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature is stirred to react 4h, obtains spinning solution, and gained spinning solution is true
Empty deaeration 20min, then by the spinning solution after deaeration after centrifugal spinning is washed 5 times, then after drawing-off, curling, in temperature be 90
It dries to constant weight, is discharged to get fibroin albumen sodium alginate composite fiber under the conditions of DEG C.The phosphatide is soybean lecithin.Institute
Monosaccharide is stated as glucose.The carbomer is Acritamer 940.
Example 5
It is 1 in mass ratio by carbomer and water：It is 75 DEG C then at temperature in standing swelling for 24 hours under room temperature after 35 mixing,
Under the conditions of rotating speed is 300r/min, heating stirring dissolving obtains carbomer liquid；It is 1 in mass ratio by fibroin albumen and water：50 mixing
It pours into beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, be 80 DEG C in temperature, rotating speed is 500r/min conditions
Under, after constant temperature stirring and dissolving 2h, material in beaker is poured into the bag filter that molecular cut off is 12kDa, and bag filter is put
In deionized water, dialyse 6 days, change a water every 5h during dialysis, when dialysis terminate after rotating speed be 12000r/min items
10min is centrifuged under part, supernatant liquor is collected, obtains pretreatment silk fibroin protein solution；By elastoser and pretreatment fibroin
Protein solution is 1 in mass ratio：Three-necked flask is poured into 600 mixing, and adjusts material pH in three-necked flask with triethanolamine solution
It tests the speed constant temperature blender with magnetic force to 7.8, then by three-necked flask immigration digital display, is 45 DEG C in temperature, rotating speed is 600r/min conditions
Under, after constant temperature stirring enzymolysis 5h, 95 DEG C are warming up to, enzyme deactivation 15min is kept the temperature, after naturally cool to room temperature, obtains enzymolysis liquid；By weight
Number meter, takes 10 parts of phosphatide successively, 8 parts of sodium alginates, 4 parts of plants essential oils, and 120 parts of enzymolysis liquids first mix phosphatide and enzymolysis liquid
It is 55kHz in supersonic frequency, temperature is ultrasonic disperse 60min under the conditions of 55 DEG C, obtains dispersion liquid, and dispersion liquid is moved into after conjunction
In reaction kettle, then sodium alginate, plants essential oil are sequentially added into the reaction kettle for fill dispersion liquid, in temperature be 100 DEG C, rotating speed
Under the conditions of 800r/min, constant temperature is stirred to react 4h, obtains reaction solution；It is again 3 in mass ratio by gained reaction solution and carbomer liquid：
It it is 80 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature is stirred to react 4h, obtains spinning solution, and gained is spun after 1 mixing
Silk liquid vacuum defoamation 20min, then by the spinning solution after deaeration after centrifugal spinning, wash 5 times, then after drawing-off, curling, Yu Wen
Spend be 90 DEG C under the conditions of dry to constant weight, discharge to get fibroin albumen sodium alginate composite fiber.The phosphatide is soybean lecithin
Fat.The plants essential oil is Lavender.The carbomer is Acritamer 940.
Example 6
It is 1 in mass ratio by carbomer and water：It is 75 DEG C then at temperature in standing swelling for 24 hours under room temperature after 35 mixing,
Under the conditions of rotating speed is 300r/min, heating stirring dissolving obtains carbomer liquid；It is 1 in mass ratio by fibroin albumen and water：50 mixing
It pours into beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, be 80 DEG C in temperature, rotating speed is 500r/min conditions
Under, after constant temperature stirring and dissolving 2h, material in beaker is poured into the bag filter that molecular cut off is 12kDa, and bag filter is put
In deionized water, dialyse 6 days, change a water every 5h during dialysis, when dialysis terminate after rotating speed be 12000r/min items
10min is centrifuged under part, supernatant liquor is collected, obtains pretreatment silk fibroin protein solution；By elastoser and pretreatment fibroin
Protein solution is 1 in mass ratio：Three-necked flask is poured into 600 mixing, and adjusts material pH in three-necked flask with triethanolamine solution
It tests the speed constant temperature blender with magnetic force to 7.8, then by three-necked flask immigration digital display, is 45 DEG C in temperature, rotating speed is 600r/min conditions
Under, after constant temperature stirring enzymolysis 5h, 95 DEG C are warming up to, enzyme deactivation 15min is kept the temperature, after naturally cool to room temperature, obtains enzymolysis liquid；By weight
Number meter, takes 10 parts of phosphatide successively, 8 parts of sodium alginates, 4 parts of monosaccharide, 4 parts of plants essential oils, 120 parts of enzymolysis liquids, first by phosphatide and
It is 55kHz in supersonic frequency after enzymolysis liquid mixing, temperature is ultrasonic disperse 60min under the conditions of 55 DEG C, obtains dispersion liquid, and will divide
Dispersion liquid is moved into reaction kettle, then sodium alginate, plants essential oil and monosaccharide, Yu Wen are sequentially added into the reaction kettle for fill dispersion liquid
It is 100 DEG C to spend, and under the conditions of rotating speed is 800r/min, constant temperature is stirred to react 4h, obtains reaction solution；By gained reaction solution vacuum defoamation
20min, then by the reaction solution after deaeration after centrifugal spinning is washed 5 times, then after drawing-off, curling, in temperature be 90 DEG C of conditions
Lower drying discharges to constant weight to get fibroin albumen sodium alginate composite fiber.The phosphatide is soybean lecithin.The monosaccharide
For glucose.The plants essential oil is Lavender.The carbomer is Acritamer 940.
1 to 6 gained fibroin albumen sodium alginate composite fiber of example is subjected to performance detection, specific detection method is as follows：
Its mechanical property is measured using LLY-06E type electronic mono-fiber strong force instruments, every test condition is respectively：Temperature is 20
DEG C, humidity 65%, tensile speed 10mm/min, clamp distance 20mm.Specific testing result is as shown in table 1：
Table 1
| Detection content | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Breaking load/（cN·dTex-1） | 2.4 | 2.0 | 2.1 | 1.8 | 1.9 | 1.8 |
| Elongation at break/% | 9.1 | 6.4 | 7.3 | 7.8 | 7.2 | 6.8 |
By 1 testing result of table it is found that present invention gained fibroin albumen sodium alginate composite fiber has good mechanical property.
Claims (7)
1. a kind of preparation method of fibroin albumen sodium alginate composite fiber, it is characterised in that specifically preparation process is：
（1）It is 1 in mass ratio by fibroin albumen and water：40~1：50 mix, and after constant temperature stirring and dissolving, are transferred to bag filter, dialysis 4
~6 days, then be centrifuged, obtain pretreatment silk fibroin protein solution；
（2）It is 1 in mass ratio by elastoser and pretreatment silk fibroin protein solution：500~1：After 600 mixing, pH is adjusted, then
It stirs and digests through constant temperature, obtain enzymolysis liquid；
（3）It counts in parts by weight, takes 8~10 parts of phosphatide, 4~8 parts of sodium alginates, 1~4 part of monosaccharide, 2~4 parts of plant essences successively
Oil, 100~120 parts of enzymolysis liquids, ultrasonic disperse after first mixing phosphatide and enzymolysis liquid, add sodium alginate, plants essential oil and
Monosaccharide, constant temperature are stirred to react, and obtain reaction solution；
（4）It is 1 in mass ratio by reaction solution and carbomer liquid：1~3：After 1 mixing, constant temperature is stirred to react, and obtains spinning solution, then pass through
Spinning after vacuum defoamation, and through washing, drawing-off, curling and drying, obtain fibroin albumen sodium alginate composite fiber.
2. a kind of preparation method of fibroin albumen sodium alginate composite fiber according to claim 1, it is characterised in that：Step
Suddenly（1）The bag filter specification is：Molecular cut off is 10~12kDa.
3. a kind of preparation method of fibroin albumen sodium alginate composite fiber according to claim 1, it is characterised in that：Step
Suddenly（2）The pH is 7.6~7.8.
4. a kind of preparation method of fibroin albumen sodium alginate composite fiber according to claim 1, it is characterised in that：Step
Suddenly（3）The phosphatide is any one in soybean lecithin or egg lecithin.
5. a kind of preparation method of fibroin albumen sodium alginate composite fiber according to claim 1, it is characterised in that：Step
Suddenly（3）The monosaccharide is any one in glucose, fructose or galactolipin.
6. a kind of preparation method of fibroin albumen sodium alginate composite fiber according to claim 1, it is characterised in that：Step
Suddenly（3）The plants essential oil is any one in Lavender, tea tree ethereal oil or camellia flower essential oil.
7. a kind of preparation method of fibroin albumen sodium alginate composite fiber according to claim 1, it is characterised in that：Step
Suddenly（4）The carbomer liquid configuration process is：It is 1 in mass ratio by carbomer and water：30~1：After 35 mixing, swelling 20 is stood
~for 24 hours, then heated stirring and dissolving, obtain carbomer liquid；The carbomer is Acritamer 940, Carbopol 941 or carbomer 937
In any one.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711278052.5A CN108193311A (en) | 2017-12-06 | 2017-12-06 | A kind of preparation method of fibroin albumen sodium alginate composite fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711278052.5A CN108193311A (en) | 2017-12-06 | 2017-12-06 | A kind of preparation method of fibroin albumen sodium alginate composite fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108193311A true CN108193311A (en) | 2018-06-22 |
Family
ID=62573866
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711278052.5A Pending CN108193311A (en) | 2017-12-06 | 2017-12-06 | A kind of preparation method of fibroin albumen sodium alginate composite fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108193311A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108914368A (en) * | 2018-07-24 | 2018-11-30 | 高昕文 | A kind of preparation method of facial mask fabric nonwoven cloth |
| CN108951159A (en) * | 2018-07-11 | 2018-12-07 | 黄勇 | A kind of textile softener |
| CN109231851A (en) * | 2018-08-09 | 2019-01-18 | 苗霞明 | A kind of mould-proof agent for glass |
| CN109512577A (en) * | 2018-10-08 | 2019-03-26 | 武汉纺织大学 | It is a kind of to promote to be cured formula biological environmental production class medical dressing and its manufacturing method |
| CN109652231A (en) * | 2018-10-29 | 2019-04-19 | 王景硕 | A kind of reactive dye soaping agent |
| CN114437246A (en) * | 2022-02-18 | 2022-05-06 | 山东海基生物科技有限公司 | Method for improving viscosity of sodium alginate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5166231A (en) * | 1990-03-27 | 1992-11-24 | Korea Research Institute Of Chemical Technology | Resin composition having biodegradability and high absorbency, nonwoven fabric made of the same and pads comprising said fabric |
| CN101358382A (en) * | 2008-08-26 | 2009-02-04 | 东华大学 | Antibacterial nano fiber material and preparation method thereof |
| CN103436986A (en) * | 2013-08-01 | 2013-12-11 | 湖州珠力纳米材料科技开发有限公司 | Preparation method of polypeptide soybean protein complex fiber |
| CN103806123A (en) * | 2014-03-03 | 2014-05-21 | 武汉理工大学 | Silk fibroin/sodium alginate composite fiber and preparation method thereof |
| CN106435815A (en) * | 2016-09-20 | 2017-02-22 | 大连工业大学 | Chemical crosslinking modified silk fibroin/alginate complex fiber and preparation method thereof |
-
2017
- 2017-12-06 CN CN201711278052.5A patent/CN108193311A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5166231A (en) * | 1990-03-27 | 1992-11-24 | Korea Research Institute Of Chemical Technology | Resin composition having biodegradability and high absorbency, nonwoven fabric made of the same and pads comprising said fabric |
| CN101358382A (en) * | 2008-08-26 | 2009-02-04 | 东华大学 | Antibacterial nano fiber material and preparation method thereof |
| CN103436986A (en) * | 2013-08-01 | 2013-12-11 | 湖州珠力纳米材料科技开发有限公司 | Preparation method of polypeptide soybean protein complex fiber |
| CN103806123A (en) * | 2014-03-03 | 2014-05-21 | 武汉理工大学 | Silk fibroin/sodium alginate composite fiber and preparation method thereof |
| CN106435815A (en) * | 2016-09-20 | 2017-02-22 | 大连工业大学 | Chemical crosslinking modified silk fibroin/alginate complex fiber and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 王景文: "《壳聚糖-天然精油防水复合膜的制备与表征》", 《中国优秀硕士学位论文全文数据库》 * |
| 郭慧玲等: "《药剂学》", 28 February 2014, 中山大学出版社 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108951159A (en) * | 2018-07-11 | 2018-12-07 | 黄勇 | A kind of textile softener |
| CN108914368A (en) * | 2018-07-24 | 2018-11-30 | 高昕文 | A kind of preparation method of facial mask fabric nonwoven cloth |
| CN109231851A (en) * | 2018-08-09 | 2019-01-18 | 苗霞明 | A kind of mould-proof agent for glass |
| CN109512577A (en) * | 2018-10-08 | 2019-03-26 | 武汉纺织大学 | It is a kind of to promote to be cured formula biological environmental production class medical dressing and its manufacturing method |
| CN109512577B (en) * | 2018-10-08 | 2022-02-18 | 武汉纺织大学 | Healing-promoting biological environment-friendly medical dressing and manufacturing method thereof |
| CN109652231A (en) * | 2018-10-29 | 2019-04-19 | 王景硕 | A kind of reactive dye soaping agent |
| CN114437246A (en) * | 2022-02-18 | 2022-05-06 | 山东海基生物科技有限公司 | Method for improving viscosity of sodium alginate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108193311A (en) | A kind of preparation method of fibroin albumen sodium alginate composite fiber | |
| Freddi et al. | Silk fibroin/cellulose blend films: preparation, structure, and physical properties | |
| Zhang et al. | Gelatin nanofibrous membrane fabricated by electrospinning of aqueous gelatin solution for guided tissue regeneration | |
| Ha et al. | Dissolution of Bombyx m ori silk fibroin in the calcium nitrate tetrahydrate− methanol system and aspects of wet spinning of fibroin solution | |
| Silva et al. | Genipin‐modified silk‐fibroin nanometric nets | |
| Qin et al. | Gelation behavior of cellulose in NaOH/urea aqueous system via cross-linking | |
| CN104790216B (en) | A kind of preparation method of the folic acid functionalized nano-fiber for target capture cancer cell | |
| CN112316914B (en) | Silk fibroin micro-nano fiber microsphere and preparation method and application thereof | |
| CN110344131B (en) | Sericin modified regenerated cellulose fiber and preparation method thereof | |
| Faragò et al. | A dry powder formulation from silk fibroin microspheres as a topical auto-gelling device | |
| CN103074700B (en) | Method for preparing filaments and staple fibers by using straw cellulose | |
| CN113136053B (en) | Preparation method of lignocellulose three-component double-crosslinking gel, gel and application | |
| CN101864081A (en) | New method for preparing polyaspartic acid hydrogels | |
| CN107118361B (en) | Silk fibroin/carboxymethyl chitosan composite gel and preparation method thereof | |
| CN106243366B (en) | A kind of preparation method of reversible thixotroping silk fibroin hydrogel | |
| CN106835367A (en) | A kind of cross-linked polysaccharides fiber and preparation method thereof | |
| CN113289050B (en) | Hemostatic sponge and preparation method thereof | |
| CN108785752A (en) | Fibroin albumen based porous materials and preparation method thereof | |
| CN106084259B (en) | A kind of preparation method of cellulose aquagel | |
| CN112999402A (en) | Electrostatic spinning gel fiber membrane and preparation method and application thereof | |
| CN108085973A (en) | A kind of nti-freckle silk mask of high-moisture-retention | |
| CN112480469A (en) | Marine organism polysaccharide-based composite sponge and preparation method and application thereof | |
| Mahsood et al. | Novel materials for moist wound management: Alginate-psyllium hybrid fibres | |
| CN110423363A (en) | A kind of preparation method and applications of high intensity superelevation elastic force hydrogel | |
| Ni et al. | Edible pullulan enhanced water-soluble keratin with improved sizing performance for sustainable textile industry |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180622 |
|
| RJ01 | Rejection of invention patent application after publication |