CN108385396A - A kind of preparation method of collagen-based carbon fiber sizing agent - Google Patents
A kind of preparation method of collagen-based carbon fiber sizing agent Download PDFInfo
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- CN108385396A CN108385396A CN201810199213.XA CN201810199213A CN108385396A CN 108385396 A CN108385396 A CN 108385396A CN 201810199213 A CN201810199213 A CN 201810199213A CN 108385396 A CN108385396 A CN 108385396A
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- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
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Abstract
The present invention relates to a kind of preparation methods of collagen-based carbon fiber sizing agent, belong to sizing agent preparing technical field.The present invention is using collagen-rich sheepskin as raw material, the boiling after acid steeps, and it is blended to obtain mixing suspension with zeolite powder after concentrating water cooking liquid, fermentation is blended in mixing suspension and the mouldy object of biomass again, obtain tunning, carbon fiber sizing agent finally is prepared in tunning and modified polyether sulphone resin and acrylic resin blending reaction, carbon fiber sizing agent produced by the present invention is good using rear wearability, good and high resilience, has broad application prospects with carbon fiber substrate caking property.
Description
Technical field
The present invention relates to a kind of preparation methods of collagen-based carbon fiber sizing agent, belong to sizing agent preparing technical field.
Background technology
Carbon fiber has excellent mechanical property, is known as the new material of 21 century.Because it is with modulus height, intensity
Greatly, proportion is small, high temperature resistant, a series of excellent performances, the composite material formed with advanced resin such as antifatigue, anticorrosive exist
The fields such as modern aerospace sophisticated technology field and Leisure Sport articles for use, civil construction, electronic product, medical instrument have extensively
General application.
But carbon fiber is fragile material, in production and process, is easy fluffing through mechanical friction, or occur single
Phenomena such as silk fracture, make the strength reduction of carbon fiber.Moreover, because the presence of lousiness, resin matrix cannot fully soak carbon fiber
Dimension easy tos produce hole, to influence the mechanical property of composite material in composite material preparation.Currently, being carried out to carbon fiber
Starching processing is the main method to solve the above problems.Starching is exactly that one layer of protection is applied on surface treated carbon fiber surface
Layer, basic composition is organic matter, thickness is about tens to hundreds of nanometers, and mass fraction is generally between 0.8%~1.5%.One
As think the main function of sizing agent be reduce fibre pick fracture of wire phenomenon, make carbon fiber boundling, improve its processing performance and rise
To protective effect.
But that there are wear-resisting properties is bad for traditional carbon fibres sizing agents at present, is bonded using between process and carbon fiber substrate
Property difference and the solidification of upper pulp layer after spring back the insufficient defect of toughness, because a kind of wearability of the invention is good, bonded with carbon fiber substrate
Property good and high resilience carbon fiber sizing agent there is positive meaning.
Invention content
Present invention mainly solves the technical issues of, for current traditional carbon fibres sizing agent, that there are wear-resisting properties is bad,
Using the insufficient defect of toughness is sprung back after bad adhesion between process and carbon fiber substrate and the solidification of upper pulp layer, a kind of glue is provided
The preparation method of former base carbon fiber sizing agent.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of collagen-based carbon fiber sizing agent, it is characterised in that specifically preparation process is：
（1）It weighs fresh sheepskin to crush, obtains sheepskin fragment, then the acetum that sheepskin fragment and mass fraction are 15% is mixed
It is standing and soak for 1~2h after conjunction, is separated by filtration to obtain filter residue after immersion, pours into reaction kettle, boils after filter residue and water are mixed
System；
（2）It after waiting for above-mentioned cooking, is separated by filtration to obtain filtrate, obtained filtrate is fitted into concentrated by rotary evaporation instrument, revolving is dense
Contracting obtains concentrate, takes zeolite to be put into ball grinder after grinding and crosses 200 mesh sieve, the zeolite powder being sieved, by zeolite powder
20~30min of stirring obtains mixing suspension after being mixed with concentrate, spare；
（3）It weighs lemon, egg yolk and sucrose to be mixed to obtain mixed liquor, mixed liquor is fitted into stainless steel pallet, and is put
Enter in greenhouse, stands mouldy 3~5 days, obtain mouldy object；
（4）Will above-mentioned mouldy object and spare mixing suspension mix after is fitted into fermentation tank, stir 20 with no bacteria stick~
30min is sealed by fermentation tank mouth after stirring, standing for fermentation obtains tunning after fermentation, spare；
（5）By polyethersulfone resin and petroleum ether mixed dissolution, polyethersulfone resin liquid is obtained, then polyethersulfone resin liquid and quality are divided
Number mixes for 98% concentrated sulfuric acid, and is heated to 60~70 DEG C, is stirred to react 1~2h, uses quality after being stirred to react again
The sodium hydroxide solution that score is 30% adjusts pH to neutrality, obtains modified polyether sulphone resin；
（6）It counts in parts by weight, weighs 10~20 parts of above-mentioned modified polyether sulphone resins, 30~40 parts of acrylic acid, 1~2 part of February
Dilaurylate, 5~10 parts of spare tunnings, 100~150 parts of deionized waters, 3~6 parts of soybean lecithins and 8~10 parts
Neopelex pours into reaction kettle successively, and 80~90 are heated under conditions of pressure is 1.2~1.4MPa
DEG C, discharging is to get collagen-based carbon fiber sizing agent after insulated and stirred reacts 15~20min.
Step（1）Described in sheepskin fragment and mass fraction be 15% the mass ratio of acetum be 1:5, filter residue and
The mass ratio of water is 1:8, the temperature of cooking is 80~90 DEG C, and the time of cooking is 1~2h.
Step（2）Described in the temperature of concentrated by rotary evaporation be 50~60 DEG C, time of concentrated by rotary evaporation is 40~50min, boiling
The mass ratio of stone powder and concentrate is 1:10.
Step（3）Described in lemon, egg yolk and sucrose mass ratio be 1:2:1, the temperature in greenhouse is 30~40 DEG C,
Relative air humidity is 60~70 DEG C.
Step（4）Described in mouldy object and suspension mixed mass ratio be 1:5, the temperature of standing for fermentation is 35~45
DEG C, the time of standing for fermentation is 5~7 days.
Step（5）Described in polyethersulfone resin and petroleum ether mass ratio be 1:10.
The beneficial effects of the invention are as follows：
（1）The present invention is using collagen-rich sheepskin as raw material, the boiling after acid steeps, and after water cooking liquid is concentrated and zeolite
Admixture of powder obtains mixing suspension, then fermentation is blended in mixing suspension and the mouldy object of biomass, obtains tunning, finally
Carbon fiber sizing agent, present invention profit is prepared in tunning and modified polyether sulphone resin and acrylic resin blending reaction
First make biomass material lemon, egg yolk and sucrose mouldy with hot and humid environment, then by mouldy object and sheepskin and zeolite powder
Fermentation is blended in last mixed liquor, due to containing abundant sheepskin collagen in the sheepskin used in the present invention, by itself and zeolite powder
Acid is produced by microbial fermentation, the basic group of sheepskin collagen peptide chain can be in conjunction with upper acid, in conjunction with the sheepskin tropocollagen molecule after upper acid
Between and the ionic cross-linked bond and hydrogen bond of interchain will be opened, sheepskin tropocollagen molecule will crosslink with acrylic acid and be formed by curing three
Netted cross-linked structure is tieed up, since the stress received can be carried out transmission dispersion by cross-linked structure, plays the work of buffering
With, therefore the rebound toughness that sizing agent uses rear material surface can be improved；
（2）The present invention is also added into the mouldy object of biomass as raw material, and biomass material is degraded using microorganism, generates big
The active group for measuring free property obtains the fermentate rich in free property active group, uses fermentate as sizing agent raw material, can be with
Active group is introduced into sizing agent, these active groups can generate hydrogen bond with the group for the carbon fiber surface for waiting for starching after use
Absorption and other Chemical bondings, the generation of these Hydrogen Binding Adsorption power and Chemical bonding can improve sizing agent and carbon fiber it
Between internal bond strength, to improve the caking property between sizing agent and carbon fiber, while the present invention also draws into sizing agent
Abrasion-proof mineral matter zeolite powder is entered, its introducing is also improved the wearability of the sizing agent film layer after solidification, has wide
Wealthy application prospect.
Specific implementation mode
Weigh fresh sheepskin and be put into tissue pulverizer 20~30min of crushing, obtain sheepskin fragment, then by sheepskin fragment and
The acetum that mass fraction is 15% is 1 in mass ratio:It is standing and soak for 1~2h after 5 mixing, is separated by filtration after immersion
It is 1 in mass ratio by filter residue and water to filter residue:It is poured into reaction kettle after 8 mixing, 1~2h of heat preservation cooking at 80~90 DEG C；It waits for
It after cooking, is separated by filtration to obtain filtrate, obtained filtrate is fitted into concentrated by rotary evaporation instrument, the concentrated by rotary evaporation at 50~60 DEG C
40~50min obtains concentrate, takes zeolite to be put into ball grinder after grinding and crosses 200 mesh sieve, the zeolite powder being sieved will boil
Stone powder and concentrate are 1 in mass ratio:20~30min of stirring obtains mixing suspension after 10 mixing, spare；It is in mass ratio
1:2:1, which weighs lemon, egg yolk and sucrose, is mixed to obtain mixed liquor, and mixed liquor is fitted into stainless steel pallet, and is put into
Temperature is 30~40 DEG C, in the greenhouse that relative air humidity is 60~70 DEG C, stands mouldy 3~5 days, obtains mouldy object；It will hair
Mould object and spare mixing suspension are 1 in mass ratio:It is fitted into fermentation tank after 5 mixing, 20~30min is stirred with no bacteria stick,
It is sealed by fermentation tank mouth after stirring, is left to ferment 5~7 days at 35~45 DEG C, obtains tunning after fermentation, it is standby
With；It is 1 in mass ratio by polyethersulfone resin and petroleum ether:10 mixed dissolutions, obtain polyethersulfone resin liquid, then by polyethersulfone resin
The concentrated sulfuric acid that liquid and mass fraction are 98% is 10 in mass ratio:1 mixing, and is heated to 60~70 DEG C, it is stirred to react 1~
2h uses the sodium hydroxide solution that mass fraction is 30% to adjust pH to neutrality, obtains modified poly (ether-sulfone) tree again after being stirred to react
Fat；It counts in parts by weight, weighs 10~20 parts of above-mentioned modified polyether sulphone resins, 30~40 parts of acrylic acid, 1~2 part of tin dilaurate
Dibutyl tin, 5~10 parts of spare tunnings, 100~150 parts of deionized waters, 3~6 parts of soybean lecithins and 8~10 part 12
Sodium alkyl benzene sulfonate pours into reaction kettle successively, and 80~90 DEG C are heated under conditions of pressure is 1.2~1.4MPa, protects
Discharging is to get collagen-based carbon fiber sizing agent after temperature is stirred to react 15~20min.
Example 1
It weighs fresh sheepskin and is put into tissue pulverizer and crush 20min, obtain sheepskin fragment, then by sheepskin fragment and mass fraction
Acetum for 15% is 1 in mass ratio:It is standing and soak for 1h after 5 mixing, is separated by filtration to obtain filter residue after immersion, will filter
Slag and water are 1 in mass ratio:It is poured into reaction kettle after 8 mixing, the heat preservation cooking 1h at 80 DEG C；It waits after cooking, filtering point
From filtrate is obtained, obtained filtrate is fitted into concentrated by rotary evaporation instrument, concentrated by rotary evaporation 40min obtains concentrate at 50 DEG C, takes boiling
Stone, which is put into ball grinder after grinding, crosses 200 mesh sieve, and zeolite powder and concentrate are by the zeolite powder being sieved in mass ratio
1:Stirring 20min obtains mixing suspension after 10 mixing, spare；It is 1 in mass ratio:2:1, which weighs lemon, egg yolk and sucrose, mixes
Conjunction stirs to get mixed liquor, and mixed liquor is fitted into stainless steel pallet, and it is 30 DEG C to be put into temperature, and relative air humidity is 60 DEG C
Greenhouse in, stand mouldy 3 days, obtain mouldy object；It is 1 in mass ratio by mouldy object and spare mixing suspension:After 5 mixing
It is fitted into fermentation tank, stirs 20min with no bacteria stick, be sealed by fermentation tank mouth after stirring, be left to ferment 5 days at 35 DEG C, send out
Tunning is obtained after ferment, it is spare；It is 1 in mass ratio by polyethersulfone resin and petroleum ether:10 mixed dissolutions, obtain polyethers
Sulphone resin liquid, then by the concentrated sulfuric acid that polyethersulfone resin liquid and mass fraction are 98% be 10 in mass ratio:1 mixing, and heat temperature raising
To 60 DEG C, it is stirred to react 1h, the sodium hydroxide solution that mass fraction is 30% is used to adjust pH to neutrality after being stirred to react again,
Obtain modified polyether sulphone resin；It counts in parts by weight, weighs 10 parts of above-mentioned modified polyether sulphone resins, 30 parts of acrylic acid, 1 part of February
Dilaurylate, 5 parts of spare tunnings, 100 parts of deionized waters, 3 parts of soybean lecithins and 8 parts of neopelexes
It pours into reaction kettle successively, 80 DEG C is heated under conditions of pressure is 1.2MPa, is gone out after insulated and stirred reaction 15min
Material is to get collagen-based carbon fiber sizing agent.
Example 2
It weighs fresh sheepskin and is put into tissue pulverizer and crush 25min, obtain sheepskin fragment, then by sheepskin fragment and mass fraction
Acetum for 15% is 1 in mass ratio:It is standing and soak for 1h after 5 mixing, is separated by filtration to obtain filter residue after immersion, will filter
Slag and water are 1 in mass ratio:It is poured into reaction kettle after 8 mixing, the heat preservation cooking 1h at 85 DEG C；It waits after cooking, filtering point
From filtrate is obtained, obtained filtrate is fitted into concentrated by rotary evaporation instrument, concentrated by rotary evaporation 45min obtains concentrate at 55 DEG C, takes boiling
Stone, which is put into ball grinder after grinding, crosses 200 mesh sieve, and zeolite powder and concentrate are by the zeolite powder being sieved in mass ratio
1:Stirring 25min obtains mixing suspension after 10 mixing, spare；It is 1 in mass ratio:2:1, which weighs lemon, egg yolk and sucrose, mixes
Conjunction stirs to get mixed liquor, and mixed liquor is fitted into stainless steel pallet, and it is 35 DEG C to be put into temperature, and relative air humidity is 65 DEG C
Greenhouse in, stand mouldy 4 days, obtain mouldy object；It is 1 in mass ratio by mouldy object and spare mixing suspension:After 5 mixing
It is fitted into fermentation tank, stirs 25min with no bacteria stick, be sealed by fermentation tank mouth after stirring, be left to ferment 6 days at 40 DEG C, send out
Tunning is obtained after ferment, it is spare；It is 1 in mass ratio by polyethersulfone resin and petroleum ether:10 mixed dissolutions, obtain polyethers
Sulphone resin liquid, then by the concentrated sulfuric acid that polyethersulfone resin liquid and mass fraction are 98% be 10 in mass ratio:1 mixing, and heat temperature raising
To 65 DEG C, it is stirred to react 1h, the sodium hydroxide solution that mass fraction is 30% is used to adjust pH to neutrality after being stirred to react again,
Obtain modified polyether sulphone resin；It counts in parts by weight, weighs 15 parts of above-mentioned modified polyether sulphone resins, 35 parts of acrylic acid, 1 part of February
Dilaurylate, 8 parts of spare tunnings, 130 parts of deionized waters, 5 parts of soybean lecithins and 9 parts of neopelexes
It pours into reaction kettle successively, 85 DEG C is heated under conditions of pressure is 1.3MPa, is gone out after insulated and stirred reaction 18min
Material is to get collagen-based carbon fiber sizing agent.
Example 3
It weighs fresh sheepskin and is put into tissue pulverizer and crush 30min, obtain sheepskin fragment, then by sheepskin fragment and mass fraction
Acetum for 15% is 1 in mass ratio:It is standing and soak for 2h after 5 mixing, is separated by filtration to obtain filter residue after immersion, will filter
Slag and water are 1 in mass ratio:It is poured into reaction kettle after 8 mixing, the heat preservation cooking 2h at 90 DEG C；It waits after cooking, filtering point
From filtrate is obtained, obtained filtrate is fitted into concentrated by rotary evaporation instrument, concentrated by rotary evaporation 50min obtains concentrate at 60 DEG C, takes boiling
Stone, which is put into ball grinder after grinding, crosses 200 mesh sieve, and zeolite powder and concentrate are by the zeolite powder being sieved in mass ratio
1:Stirring 30min obtains mixing suspension after 10 mixing, spare；It is 1 in mass ratio:2:1, which weighs lemon, egg yolk and sucrose, mixes
Conjunction stirs to get mixed liquor, and mixed liquor is fitted into stainless steel pallet, and it is 40 DEG C to be put into temperature, and relative air humidity is 70 DEG C
Greenhouse in, stand mouldy 5 days, obtain mouldy object；It is 1 in mass ratio by mouldy object and spare mixing suspension:After 5 mixing
It is fitted into fermentation tank, stirs 30min with no bacteria stick, be sealed by fermentation tank mouth after stirring, be left to ferment 7 days at 45 DEG C, send out
Tunning is obtained after ferment, it is spare；It is 1 in mass ratio by polyethersulfone resin and petroleum ether:10 mixed dissolutions, obtain polyethers
Sulphone resin liquid, then by the concentrated sulfuric acid that polyethersulfone resin liquid and mass fraction are 98% be 10 in mass ratio:1 mixing, and heat temperature raising
To 70 DEG C, it is stirred to react 2h, the sodium hydroxide solution that mass fraction is 30% is used to adjust pH to neutrality after being stirred to react again,
Obtain modified polyether sulphone resin；It counts in parts by weight, weighs 20 parts of above-mentioned modified polyether sulphone resins, 40 parts of acrylic acid, 2 parts of February
Dilaurylate, 10 parts of spare tunnings, 150 parts of deionized waters, 6 parts of soybean lecithins and 10 parts of dodecyl benzene sulfonic acid
Sodium pours into reaction kettle successively, and 90 DEG C are heated under conditions of pressure is 1.4MPa, is gone out after insulated and stirred reaction 20min
Material is to get collagen-based carbon fiber sizing agent.
Reference examples
With the carbon fiber sizing agent example as a contrast of company of Beijing production
After using the carbon fiber sizing agent starching in fiber and reference examples after carbon fiber sizing agent starching produced by the present invention
Fiber carry out performance detection, testing result is as shown in table 1：
1 performance test results of table
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Harness intensity（GPa） | 7.0 | 6.9 | 6.9 | 6.6 |
| Single fiber elasticity modulus（GPa） | 345 | 345 | 345 | 333 |
| Tensile strength（MPa） | 162 | 163 | 165 | 148 |
| Bending strength（MPa） | 213 | 218 | 220 | 201 |
| Impact strength（KJ/m2） | 23 | 25 | 28 | 19 |
Carbon fiber sizing agent produced by the present invention is good using rear wearability it can be seen from detection data in upper table, with carbon fiber
Base bonding property is good and high resilience, has broad application prospects.
Claims (6)
1. a kind of preparation method of collagen-based carbon fiber sizing agent, it is characterised in that specifically preparation process is：
（1）It weighs fresh sheepskin to crush, obtains sheepskin fragment, then the acetum that sheepskin fragment and mass fraction are 15% is mixed
It is standing and soak for 1~2h after conjunction, is separated by filtration to obtain filter residue after immersion, pours into reaction kettle, boils after filter residue and water are mixed
System；
（2）It after waiting for above-mentioned cooking, is separated by filtration to obtain filtrate, obtained filtrate is fitted into concentrated by rotary evaporation instrument, revolving is dense
Contracting obtains concentrate, takes zeolite to be put into ball grinder after grinding and crosses 200 mesh sieve, the zeolite powder being sieved, by zeolite powder
20~30min of stirring obtains mixing suspension after being mixed with concentrate, spare；
（3）It weighs lemon, egg yolk and sucrose to be mixed to obtain mixed liquor, mixed liquor is fitted into stainless steel pallet, and is put
Enter in greenhouse, stands mouldy 3~5 days, obtain mouldy object；
（4）Will above-mentioned mouldy object and spare mixing suspension mix after is fitted into fermentation tank, stir 20 with no bacteria stick~
30min is sealed by fermentation tank mouth after stirring, standing for fermentation obtains tunning after fermentation, spare；
（5）By polyethersulfone resin and petroleum ether mixed dissolution, polyethersulfone resin liquid is obtained, then polyethersulfone resin liquid and quality are divided
Number mixes for 98% concentrated sulfuric acid, and is heated to 60~70 DEG C, is stirred to react 1~2h, uses quality after being stirred to react again
The sodium hydroxide solution that score is 30% adjusts pH to neutrality, obtains modified polyether sulphone resin；
（6）It counts in parts by weight, weighs 10~20 parts of above-mentioned modified polyether sulphone resins, 30~40 parts of acrylic acid, 1~2 part of February
Dilaurylate, 5~10 parts of spare tunnings, 100~150 parts of deionized waters, 3~6 parts of soybean lecithins and 8~10 parts
Neopelex pours into reaction kettle successively, and 80~90 are heated under conditions of pressure is 1.2~1.4MPa
DEG C, discharging is to get collagen-based carbon fiber sizing agent after insulated and stirred reacts 15~20min.
2. a kind of preparation method of collagen-based carbon fiber sizing agent according to claim 1, it is characterised in that：Step（1）
Described in sheepskin fragment and mass fraction be 15% the mass ratio of acetum be 1:5, the mass ratio of filter residue and water is 1:8,
The temperature of cooking is 80~90 DEG C, and the time of cooking is 1~2h.
3. a kind of preparation method of collagen-based carbon fiber sizing agent according to claim 1, it is characterised in that：Step（2）
Described in the temperature of concentrated by rotary evaporation be 50~60 DEG C, time of concentrated by rotary evaporation is 40~50min, zeolite powder and concentrate
Mass ratio is 1:10.
4. a kind of preparation method of collagen-based carbon fiber sizing agent according to claim 1, it is characterised in that：Step（3）
Described in lemon, egg yolk and sucrose mass ratio be 1:2:1, the temperature in greenhouse is 30~40 DEG C, and relative air humidity is
60~70 DEG C.
5. a kind of preparation method of collagen-based carbon fiber sizing agent according to claim 1, it is characterised in that：Step（4）
Described in mouldy object and suspension mixed mass ratio be 1:5, the temperature of standing for fermentation is 35~45 DEG C, standing for fermentation when
Between be 5~7 days.
6. a kind of preparation method of collagen-based carbon fiber sizing agent according to claim 1, it is characterised in that：Step（5）
Described in polyethersulfone resin and petroleum ether mass ratio be 1:10.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110656495A (en) * | 2019-10-31 | 2020-01-07 | 江苏金荣泰新材料科技有限公司 | Environment-friendly polyester filament sizing agent and sizing process |
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