CN108977930A - A kind of high strength acid resistant alkali tencel - Google Patents
A kind of high strength acid resistant alkali tencel Download PDFInfo
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- CN108977930A CN108977930A CN201810928125.9A CN201810928125A CN108977930A CN 108977930 A CN108977930 A CN 108977930A CN 201810928125 A CN201810928125 A CN 201810928125A CN 108977930 A CN108977930 A CN 108977930A
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- 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
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- 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
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- 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
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Abstract
The invention mainly relates to tencel processing technique fields, a kind of high strength acid resistant alkali tencel is disclosed, is made of raw material from the following weight: 10-15 parts of chitosan, 60-75 parts of glycidyl ester epoxy resin, 2-3 parts of carbon nanotube, 15-18 parts of nano-titanium dioxide；Fiber resistance to acid and alkali prepared by the present invention is strong, and dye stability is good, and use scope is wide.
Description
Technical field
The invention mainly relates to new special fibre processing technologies field more particularly to a kind of novel fibres of high strength acid resistant alkali
Dimension.
Background technique
It is raw material that chemical fibre, which is with natural polymer or artificial synthesized high-molecular compound, is spun by preparation
The processes such as silk stock solution, the spinning and post-processing fiber obtained with textile performance.Chemical fibre is many kinds of, and usage amount is huge
Greatly, still, in some special fields, the fiber as used in chemical plant, special equipment generally requires intensity with higher
And acid-proof alkaline, currently used corrosion resistant fiber are mostly fluorine-containing fiber or inorfil, fluorinated fiber cost is high,
Raw materials for production have toxicity, and inorfil uses high temperature wire drawing, and energy consumption is higher.
Summary of the invention
In order to make up the defect of prior art, the object of the present invention is to provide a kind of high strength acid resistant alkali tencels.
A kind of high strength acid resistant alkali tencel, is made of raw material from the following weight: 10-15 parts of chitosan, shrink are sweet
60-75 parts of grease based epoxy resin, 2-3 parts of carbon nanotube, 15-18 parts of nano-titanium dioxide；
The carbon nanotube uses after following processing: a, carbon nanotube and the sodium hydroxide solution of 2mol/L will be used to soak
It steeps, is stirred continuously in soaking process, is then washed to neutrality using deionized water；
B, the carbon nanotube after washing is impregnated using the acetic acid solution of 1mol/L, in soaking process, at ultrasonic oscillation
15-20min is managed, is dried at 50 DEG C, then prepares treatment fluid；Treatment fluid is made of following component by weight: silane coupling agent 1
Part, 0.08 part of yttrium nitrate, 2.2 parts of sodium metaphosphate, 1.2 parts of glacial acetic acid, 50 parts of water are mixed 20min, obtain treatment fluid, take
10 parts of carbon nanotube are added in above-mentioned treatment fluid, and using ultrasonication 20-30min, mixed liquor is then used vacuum rotating
Evaporator is evaporated, and obtains pretreatment carbon nanotube.Through having porous structure can after adding treatment fluid due to carbon nanotube
There is good dispersant adsorption effect to the ingredient in treatment fluid, in solution glacial acetic acid also can by chemical bonds such as hydrogen bonds and
Suction-operated is adsorbed on pore surface, promotes the complexing power of carbon nanotube and polarity or apolar substance.
The glycidyl ester epoxy resin is terephthalic acid diglycidyl ester, epoxide number 0.4-0.45mol/
100g。
The chitosan passes through modification, chitosan is added in the sodium selenite solution of 3 ~ 4 times of chitosan weight amounts,
Sodium selenite solution concentration is 40 ~ 45mg/L, is gradually heated to 55 ~ 60 DEG C, stirs evenly and be placed in vacuum rotary evaporator,
55 ~ 60 DEG C of temperature, revolving speed is 23 ~ 25 revs/min, and vacuum degree is -0.08 ~ -0.1MPa, while carrying out the intermittent photograph of ultraviolet light
It penetrates, isothermal holding 40 ~ 50 minutes, promotes selenium in conjunction with amino of chitosan, take out, it is poly- to obtain modified shell for freeze-drying to no moisture
Sugar removes extra moisture, makes blocky Chitosan powder, increases the binding ability of amino of chitosan and selenium, increases modified shell
The stability of glycan increases the flexibility and caking property of chitosan, can also be obviously improved treatment process chitosan and carbon nanometer
The effect of pipe mixing dispersion and the intensity of connection, dispersibility and compatibility in the fibre are also obviously improved, and promote the resistance to of fiber
Corrosivity and intensity.
A kind of high strength acid resistant alkali tencel, preparation method includes the following steps:
(1), raw material mixes: modification of chitosan and pretreatment carbon nanotube being mixed, mixture can increase the intensity of fiber and resistance to
Acid-base property makes fiber not decompose or be carbonized when being in high temperature, is able to maintain the shape of fiber, and modification of chitosan weight is added
Nano-titanium dioxide is added using ultrasonic oscillation 20min in the deionized water of amount 62 ~ 64%, is uniformly mixed, and glycidol is added
Esters epoxy resin and 1 times of glycidyl ester epoxy resin weight of dehydrated alcohol, after being heated to 50 ~ 55 DEG C, insulated and stirred
30 ~ 40 minutes, deaeration obtained spinning solution；
(2), spinning is washed: spinning solution being sent into spinning machine and carries out wet spinning, coagulating bath is alkaline ethanol solution, takes out and spins
It is rinsed through deionized water to neutrality after silk, obtains as-spun fibre；Ensure the fiber number of fiber, be conducive to production,
(3) dry: as-spun fibre being placed in baking oven and is dried, temperature is 23 ~ 25 DEG C, and uitraviolet intensity is 1500 μ W/
Cm2 obtains high strength acid resistant alkali tencel.The flexibility and fibre strength of fiber can be increased.
The intermittent irradiation of the ultraviolet light, exposure intensity are 2200 μ W/cm2, irradiate 10min, stop 15min.
2mol/L hydrogen is added in 68 ~ 72% alcoholic solution to volume fraction in the alkaline ethanol solution of the step (2)
Sodium hydroxide solution, the pH for being adjusted to alcoholic solution is 9.4 ~ 9.8.
Wet spinning in the step (2), spinneret 5 ~ 7m/min of speed, stretch bath temperature by 10 ~ 25 DEG C of coagulation bath temperature
45 ~ 50 DEG C, 4 ~ 5m/min of draft speed.
Fibre number is 85-110dtex.
Fiber in the application can be used for preparing pipeline corrosion protection cloth, special working suit, acid and alkali-resistance gloves etc..
The invention has the advantages that high strength acid resistant alkali tencel provided by the invention, selenous acid is added into chitosan
Sodium solution carries out vacuum rotating after being gradually heated up, and carries out the intermittent irradiation of ultraviolet light, promotes selenium in conjunction with amino of chitosan,
It is finally freeze-dried, removes extra moisture, make blocky Chitosan powder, increase the combination energy of amino of chitosan and selenium
Power increases the stability of modification of chitosan, increases the flexibility and caking property of chitosan,；By modification of chitosan and carbon nanotube
Mixing, increases the flame retardant property of fiber, makes fiber that burning will not occur when being in 200 DEG C, decompose or be carbonized, is able to maintain and does not send out
Raw apparent deformation, carbon nanotube is by being modified, and dispersion effect and the performance in conjunction with chitosan are obviously improved, carbon nanotube
Porous structure can closely be connect with modification of chitosan, significant humidification can be played, avoid in use process shell poly-
Sugar or carbon nanotube are dissolved out from fiber, are proposed HR highly reinforcing effect, are carried out insulated and stirred after adding epoxy resin, make spinning
Stoste is sufficiently swollen, and improves spinning uniformity, and the epoxy resin of addition is glycidyl ester epoxy resin, glycidol esters
Epoxy resin can be closely crosslinked with modification of chitosan and pretreatment carbon nanotube, increased the intensity of fiber, avoided using
Journey fracture, prolongs long stapled service life；Spinning parameter is adjusted when wet spinning, it is ensured that the fiber number of fiber is conducive to production；When dry into
Row low temperature drying, and irradiated with ultraviolet light, it can increase the fibre strength of fiber, and the preparation method preparation of the application
Material has dispersion and adhesion effect well, easy coloring and retention of color height to color.
Specific embodiment
Illustrate the present invention with specific embodiment below.
Embodiment 1
A kind of high strength acid resistant alkali tencel, is made of raw material from the following weight: 12 parts of chitosan, glycidol esters ring
68 parts of oxygen resin, 2.2 parts of carbon nanotube, 16.5 parts of nano-titanium dioxide；
The carbon nanotube uses after following processing: a, carbon nanotube and the sodium hydroxide solution of 2mol/L will be used to soak
It steeps, is stirred continuously in soaking process, is then washed to neutrality using deionized water；
B, the carbon nanotube after washing is impregnated using the acetic acid solution of 1mol/L, in soaking process, at ultrasonic oscillation
15-20min is managed, is dried at 50 DEG C, then prepares treatment fluid；Treatment fluid is made of following component by weight: silane coupling agent 1
Part, 0.08 part of yttrium nitrate, 2.2 parts of sodium metaphosphate, 1.2 parts of glacial acetic acid, 50 parts of water are mixed 20min, obtain treatment fluid, take
10 parts of carbon nanotube are added in above-mentioned treatment fluid, and using ultrasonication 20-30min, mixed liquor is then used vacuum rotating
Evaporator is evaporated, and obtains pretreatment carbon nanotube.
The glycidyl ester epoxy resin is terephthalic acid diglycidyl ester, epoxide number 0.42mol/
100g。
The chitosan passes through modification, chitosan is added in the sodium selenite solution of 3 ~ 4 times of chitosan weight amounts,
Sodium selenite solution concentration is 40mg/L, is gradually heated to 55 ~ 60 DEG C, stirs evenly and be placed in vacuum rotary evaporator, temperature
55 ~ 60 DEG C of degree, revolving speed are 23 ~ 25 revs/min, and vacuum degree is -0.08 ~ -0.1MPa, while carrying out the intermittent irradiation of ultraviolet light,
It isothermal holding 40 ~ 50 minutes, takes out, is freeze-dried to no moisture, obtains modification of chitosan.
Preparation method includes the following steps:
(1), raw material mix: by modification of chitosan and pretreatment carbon nanotube mix, be added modification of chitosan weight 62% go from
Nano-titanium dioxide is added using ultrasonic oscillation 20min in sub- water, is uniformly mixed, be added glycidyl ester epoxy resin and
The dehydrated alcohol that 1 times of glycidyl ester epoxy resin weight, after being heated to 50 ~ 55 DEG C, insulated and stirred 40 minutes, deaeration was obtained
Spinning solution；
(2), spinning is washed: spinning solution being sent into spinning machine and carries out wet spinning, coagulating bath is alkaline ethanol solution, takes out and spins
It is rinsed through deionized water to neutrality after silk, obtains as-spun fibre；
(3) dry: as-spun fibre being placed in baking oven and is dried, temperature is 23 ~ 25 DEG C, and uitraviolet intensity is 1500 μ W/
Cm2 obtains high strength acid resistant alkali tencel.
The intermittent irradiation of the ultraviolet light, exposure intensity are 2200 μ W/cm2, irradiate 10min, stop 15min.
2mol/L hydrogen is added in 68 ~ 72% alcoholic solution to volume fraction in the alkaline ethanol solution of the step (2)
Sodium hydroxide solution, the pH for being adjusted to alcoholic solution is 9.4 ~ 9.8.
Wet spinning in the step (2), spinneret 5 ~ 7m/min of speed, stretch bath temperature by 10 ~ 25 DEG C of coagulation bath temperature
45 ~ 50 DEG C, 4 ~ 5m/min of draft speed.
Fiber number is 85-110dtex.
Embodiment 2
A kind of high strength acid resistant alkali tencel, is made of raw material from the following weight: 15 parts of chitosan, glycidol esters ring
65 parts of oxygen resin, 2 parts of carbon nanotube, 16 parts of nano-titanium dioxide；Other methods are the same as embodiment 1.
Embodiment 3
Compared with Example 1, processing is not modified to carbon nanotube.
Embodiment 4
Compared with Example 1, processing is not modified to chitosan.
Embodiment 5
Raw material and embodiment 1 are consistent, but preparation method uses conventional wet lay spinning process.
Experiment 1
Verify mechanical property of the fiber of embodiment and comparative example preparation after acid or base extraction:
Comparative example 1
Without using chitosan, other raw materials and method are the same as embodiment 1.
Comparative example 2
Without using nano-titanium dioxide, other raw materials and method are the same as embodiment 1.
Comparative example 3
Without using carbon nanotube, other raw materials and method are the same as embodiment 1.
Comparative example 4
Without using nano-titanium dioxide and carbon nanotube.
Example and the fiber of comparative example are appropriate respectively, according to " fibre strength detection technique and instrument, Zhu Genfeng etc. "
Method, use dry strong (cN/dtex), wet strong (cN/dtex) and the soda acid of YG029-I full automatic single yarn tester detection fiber
Intensity that treated, every group repeats detection 5 times, and results are averaged, and the mechanical property of embodiment and comparative example fiber is shown in Table 1.
Table 1
Note: before test, fiber is handled using the hydrochloric acid solution of distilled water, the sodium hydroxide solution of 2mol/L and 2mol/L respectively
Then 30min is dried.
As shown in Table 1, the intensity of the fiber prepared using the application method is high, and acid-alkali-corrosive-resisting is obviously improved,
After using acid-base solution processing, fiber can still keep very high intensity.
Experiment 2
In order to verify influence of the different preparation methods to fibre property, following comparative experiments, and the mechanics of test material are set
Performance.
Comparative example 5
Without isothermal holding in when step (1) feedstock processing, other raw materials and method are the same as embodiment 1.
Comparative example 6
Spinning process uses melt spinning, other steps and embodiment 1 are consistent.
Comparative example 7
Coagulating bath uses ethanol solution, does not use alkaline ethanol solution, other steps and embodiment 1 are consistent.
As a result such as table 2:
Table 2:
As shown in Table 2, fibre strength made of the preparation method using the application is bigger, to the application technical arrangement plan
Afterwards, prepared fibre property is remarkably decreased, and illustrates that the technological parameter of the application is more excellent.
Experiment 3
The flame retardant property of embodiment and comparative example fiber:
Its limit oxygen index LOI(% is measured by GB/T5455-1997 " textile combustion performance test normal beam technique "), and use UL94
The flame retardant rating of standard detection each group fiber, and the fiber 10g of each group is taken to burn respectively, count each group fibre deformation or combustion
Critical-temperature when burning, each test are repeated 3 times, and results are averaged, and the flame retardant property of embodiment and comparative example fiber is shown in Table
2。
Table 3: the flame retardant property of embodiment and comparative example fiber
Note: "-" indicates not fire-retardant.
From table 3 the result shows that, the high strength acid resistant alkali tencel of embodiment, limit oxygen index and critical-temperature are obvious
Better than comparative example, flame retardant rating is significantly higher, illustrates that high strength acid resistant alkali tencel provided by the invention has resistance well
Fire performance.
The dyeability of embodiment and comparative example fiber:
Example and the fiber 10g of comparative example are placed in 100g reactive dyeing bath foam respectively, are heated to 45 DEG C, keep the temperature 30 points
Clock observes the colouring situation of each group fiber, as a result:
Embodiment 1, embodiment 2,5 coloring effect of embodiment are best, upper color depth, uniformly, and using 2mol/L sodium hydroxide
It is colour-fast after solution processing 30min；
Embodiment 3,4 coloring effects are taken second place, and are painted deeper, substantially uniform, and are handled using the sodium hydroxide solution of 2mol/L
It slightly fades after 30min；
Color uniformity is relatively poor on fiber in other comparative examples, fugitive color.
Claims (8)
1. a kind of high strength acid resistant alkali tencel, which is characterized in that be made of raw material from the following weight: chitosan 10-15
Part, 60-75 parts of glycidyl ester epoxy resin, 2-3 parts of carbon nanotube, 15-18 parts of nano-titanium dioxide；
The carbon nanotube uses after following processing: a, carbon nanotube and the sodium hydroxide solution of 2mol/L will be used to soak
It steeps, is stirred continuously in soaking process, is then washed to neutrality using deionized water；
B, the carbon nanotube after washing is impregnated using the acetic acid solution of 1mol/L, in soaking process, at ultrasonic oscillation
15-20min is managed, is dried at 50 DEG C, then prepares treatment fluid；Treatment fluid is made of following component by weight: silane coupling agent 1
Part, 0.08 part of yttrium nitrate, 2.2 parts of sodium metaphosphate, 1.2 parts of glacial acetic acid, 50 parts of water are mixed 20min, obtain treatment fluid, take
10 parts of carbon nanotube are added in above-mentioned treatment fluid, and using ultrasonication 20-30min, mixed liquor is then used vacuum rotating
Evaporator is evaporated, and obtains pretreatment carbon nanotube.
2. a kind of high strength acid resistant alkali tencel according to claim 1, which is characterized in that the glycidol esters
Epoxy resin is terephthalic acid diglycidyl ester, epoxide number 0.4-0.45mol/100g.
3. a kind of high strength acid resistant alkali tencel according to claim 1, which is characterized in that the chitosan is by changing
Property processing, by chitosan be added 3 ~ 4 times of chitosan weight amount sodium selenite solutions in, sodium selenite solution concentration be 40 ~
45mg/L is gradually heated to 55 ~ 60 DEG C, stirs evenly and be placed in vacuum rotary evaporator, 55 ~ 60 DEG C of temperature, revolving speed be 23 ~
25 revs/min, vacuum degree is -0.08 ~ -0.1MPa, while carrying out the intermittent irradiation of ultraviolet light, isothermal holding 40 ~ 50 minutes, is taken
Out, freeze-drying obtains modification of chitosan to no moisture.
4. a kind of high strength acid resistant alkali tencel described in one of -3 according to claim 1, which is characterized in that preparation method
The following steps are included:
(1), raw material mixes: modification of chitosan and pretreatment carbon nanotube being mixed, modification of chitosan weight 62 ~ 64% is added
Nano-titanium dioxide is added using ultrasonic oscillation 20min in deionized water, is uniformly mixed, and glycidol esters asphalt mixtures modified by epoxy resin is added
Rouge and 1 times of glycidyl ester epoxy resin weight of dehydrated alcohol, after being heated to 50 ~ 55 DEG C, insulated and stirred 30 ~ 40 minutes,
Deaeration obtains spinning solution；
(2), spinning is washed: spinning solution being sent into spinning machine and carries out wet spinning, coagulating bath is alkaline ethanol solution, takes out and spins
It is rinsed through deionized water to neutrality after silk, obtains as-spun fibre；
(3) dry: as-spun fibre being placed in baking oven and is dried, temperature is 23 ~ 25 DEG C, and uitraviolet intensity is 1500 μ W/
Cm2 obtains high strength acid resistant alkali tencel.
5. a kind of high strength acid resistant alkali tencel according to claim 3, which is characterized in that the ultraviolet light interval
Formula irradiation, exposure intensity are 2200 μ W/cm2, irradiate 10min, stop 15min.
6. a kind of high strength acid resistant alkali tencel according to claim 4, which is characterized in that the alkali of the step (2)
Property ethanol solution, to volume fraction be 68 ~ 72% alcoholic solution in be added 2mol/L sodium hydroxide solution, it is molten to be adjusted to alcohol
The pH of liquid is 9.4 ~ 9.8.
7. a kind of high strength acid resistant alkali tencel according to claim 4, which is characterized in that in the step (2)
Wet spinning, spinneret 5 ~ 7m/min of speed, stretch 45 ~ 50 DEG C of bath temperature, 4 ~ 5m/ of draft speed by 10 ~ 25 DEG C of coagulation bath temperature
min。
8. described in any item a kind of high strength acid resistant alkali tencels according to claim 1 ~ 7, which is characterized in that fibre number
For 85-110dtex.
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Application publication date: 20181211 |