CN107475807A - A kind of preparation method of the fiber of modification of nylon 6 - Google Patents
A kind of preparation method of the fiber of modification of nylon 6 Download PDFInfo
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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
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation 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
- 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
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
Abstract
The invention discloses a kind of preparation method of the fiber of modification of nylon 6, belong to spinning material field.The specific preparation method of the fiber of modification of nylon 6 prepared by the present invention is：First hydrolysis nylon 6 fiber will be made after nylon 6 fiber partial hydrolysis; then the existing principle for the different solubility in various concentrations salting liquid of the spider's thread is utilized by spider's thread fiber degradation; must be degraded spider's thread fiber; the fiber of copolymer nylon 6 is made under phosphoric acid catalyzed and nitrogen protection with degraded spider's thread fiber in hydrolysis nylon 6 fiber again; by the fiber impregnation of copolymer nylon 6 in organosilicon diethyl ether solution, stand, filter after reacting a period of time; vacuum drying, obtains the fiber of modification of nylon 6.The fiber of modification of nylon 6 prepared by the present invention can effectively improve the toughness of nylon 6 fiber, hitting property of notched Izod impact and friction stability.
Description
Technical field
The invention discloses a kind of preparation method of the fiber of modification of nylon 6, belong to spinning material field.
Background technology
Polyamide is commonly called as nylon（Nylon）, English name Polyamide（Abbreviation PA）, density 1.15g/cm3, including fat
Fat race PA, fat-aromatic series PA and aromatic series PA.Wherein aliphatic PA is wide in variety, and yield is big, is widely used, and it is named by closing
Into depending on the specific carbon number of monomer.Polyamide has a good combination property, including mechanical property, heat resistance, wear-resistant
Property, chemical proofing and self lubricity, and coefficient of friction is low, there is certain anti-flammability, it is easy to process, suitable for using glass fibre
With other filler filling enhancing modifieds, improve performance and expand application.Polyamide it is various in style, have PA6, PA66,
PA11, PA12, PA46, PA610, PA612, PA1010 etc., and the semi-aromatic nylon developed in recent years（PA6T）And special type
Many new varieties such as nylon.
PA6 is that earliest kind is developed in engineering plastics, and one of maximum kind of yield in Maranyl at present,
With excellent comprehensive such as wear-resisting, oil resistant, self-lubricating, insulation, good mechanical performance, easy-formation processing, antidetonation sound-absorbing, weak acid and alkali resistance
Close performance.But there is also the defects of dry state and low temperature notched sensitiveness are poor, and impact strength is low, make its application by a fixed limit by PA6
System.In recent years, by blending and modifying, its research developed to directions such as HI high impact, low water suction and optimization processing is made to turn into extensive
The problem of concern.It is material modified specifically how to obtain integrating the activeness and quietness of high rigidity, high intensity and high tenacity, is even more
The focus of research.PA6 tensile strength is generally 60~90MPa, and appropriate reinforcing fiber is equipped with PA6, can make its stretching
Intensity, rigidity etc. are improved significantly, while can make the dimensionally stable of product, and shrinkage factor reduces, and thermal deformation reduces.The increasing of fiber
Potent fruit depends on fiber and cohered with the firm of PA6 matrixes, load suffered by plastics is transferred on high strength fibre, and
Localised load is delivered to by whole matrix by fiber.Reinforcing fiber has glass fibre, whisker and CNT etc. at present.It is inorganic
Particle toughening PA6 effect may be good not as elastomer, but while PA6 toughness is improved, can also improve other mechanical properties.
But due to its toughening effect unobvious, therefore seldom it is used alone.
Polyamide（PA）The effect of the particularity of material molecule chain structure and contained polar group, make its dry friction
Coefficient is higher, and friction stability is poor, limits use of the polyamide on tribology part, therefore need badly and it is modified
To expand its application in tribological field.It is current raising polyamide mechanical strength by adding high performance kollag
Include graphite, MoS with one of the effective way of anti-wear performance conventional kollag2, polytetrafluoroethylene (PTFE)（PTFE）And superelevation
Molecular weight polyethylene（UHMWPE）PA6 tribology can be improved to varying degrees Deng these conventional kollags
Can, but its effect is all unsatisfactory.
Therefore, solve the problem of PA6 friction stabilities are poor, and notch impact strength is low, toughness deficiency, turn into improvement tradition
The only way which must be passed of PA6 performances.
The content of the invention
The present invention solves the technical problem of：Poor, the notch impact strength for the fibre frictoin stability of conventional nylon 6
It is low, the problem of toughness deficiency, there is provided a kind of preparation method of the fiber of modification of nylon 6.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of the fiber of modification of nylon 6, specific preparation process are：
（1）By nylon 6 fiber and water in mass ratio 1：50 mixing, constant temperature and pressure react 10~15min, filter, and dry, must hydrolyze
Nylon 6 fiber；
（2）By spider's thread fiber and salting liquid in mass ratio 2：5 are put into beaker, mix 40~60min, add salting liquid
The water that 15~20 times of quality, filtered after being uniformly mixed, filtrate is concentrated, dried, must degrade spider's thread fiber；
（3）Will hydrolysis nylon 6 fiber and water in mass ratio 10：1 mixing, sequentially add hydrolysis nylon 6 fiber quality 0.4~
0.6 times of phosphoric acid solution, the organic acid soln of 0.3~0.5 times of hydrolysis nylon 6 fiber quality, under the protection of nitrogen, decompression is permanent
Warm stirring reaction, then heat up, and the degraded spider's thread fiber of 0.4~0.6 times of hydrolysis nylon 6 fiber quality is added, it is permanent to continue constant temperature
Pressure 6~8h of reaction, cools down, filtering, obtains filter cake；
（4）By organosilicon and ether in mass ratio 1：30 mixing, obtain organosilicon diethyl ether solution, filter cake are impregnated in into organosilicon ether
In solution, the catalyst of 0.1~0.3 times of filter cake quality is added, after 50~60min of stirring reaction, stand, filtering, vacuum is done
It is dry, produce the fiber of modification of nylon 6.
Step（2）The thiocyanic acid that described salting liquid is the lithium-bromide solution that mass fraction is 85% or mass fraction is 85%
Any one in lithium solution.
Step（3）Described organic acid soln is the ethanedioic acid solution that mass fraction is 20~40% or mass fraction is 20
Any one in~40% acetum.
Step（4）Described organosilicon is any one in benzyl silane or diphenyl silane.
Step（4）Described catalyst is any one in anhydrous magnesium sulfate or dead plaster.
The beneficial effects of the invention are as follows：
（1）Technical solution of the present invention is copolymerized using spider's thread fiber molecule and nylon 6 fiber molecule, and one side spider's thread fiber molecule is inhaled
Attached property is stronger, after being copolymerized with nylon 6 fiber molecule, the enhancing of nylon 6 fiber intermolecular force, makes the macromolecular chain of nylon 6 steady
Qualitative increase, so that nylon 6 fiber friction stability and notched-impact resistance are improved, while the spider's thread fiber molecule being copolymerized
There is excellent elasticity again, make the nylon 6 fiber after copolymerization that there is preferably elasticity, another aspect spider's thread fiber molecule, which has, to be dredged
The beta structure of water, after being copolymerized with nylon 6 fiber molecule, molecule of the nylon 6 fiber macromolecular chain due to combining this structure,
Therefore hydrophobicity is improved, and is improved so as to the hydrolysis resistance of nylon 6 fiber；
（2）Nylon 6 fiber after copolymerization is impregnated in organic silicon solution by technical solution of the present invention, the nylon after being on the one hand copolymerized
6 fiber moieties sections are the small molecule section after spider's thread degraded, and the small molecule section surface carries more active group, has good
Good absorption property, the organosilicon in system can be adsorbed, in the presence of catalyst, intermolecular generation dehydrating condensation forms silicon
Oxygen key, silicon oxygen bond are larger due to bond energy, it is not easy to are broken, the hydrolytic resistance and mechanical performance for making nylon 6 fiber are entered
One step is lifted, and on the other hand, Long carbon chain molecule is carried in the silicon oxygen bond other end of nylon 6 fiber strand absorption, fine in nylon 6
Tie up in application process, Long carbon chain molecule can form one layer of hydrophobic protective layer on nylon 6 fiber macromolecular chain surface, avoid nylon
While 6 fiber molecules hydrolyze, the stability of nylon 6 fiber macromolecular chain is further improved, makes nylon 6 fiber hydrophobicity and rubs
Stability is wiped to improve.
Embodiment
First by nylon 6 fiber and water in mass ratio 1：50 add in stainless steel cauldron, are 280~300 DEG C in temperature, press
Under conditions of power is 8~10MPa, constant temperature and pressure filters after reacting 10~15min, obtains No. 1 filtrate, by No. 1 filtrate, and by gained
No. 1 filtrate is transferred to Rotary Evaporators, in temperature be 45~50 DEG C, pressure be 600~800Pa under the conditions of, vacuum rotary steam concentration 4~
6h, concentrate is obtained, by concentrate vacuum freeze drying, obtain hydrolysis nylon 6 fiber；It is 85% by spider's thread fiber and mass fraction
Salting liquid in mass ratio 2：5 are put into beaker, by beaker move into digital display temperature constant magnetic stirring instrument in, in temperature be 35~40 DEG C,
Under conditions of rotating speed is 350~500r/min, constant temperature 40~60min of stirring reaction, under stirring, added into beaker
The water that 15~20 times of salting liquid quality, after continuation constant temperature is stirred 10~15min, beaker is stood into 1~2h, filtering, obtains No. 1
Filter cake, by No. 1 filter cake be put into vacuum it is dry and cold freeze it is dry, must degrade spider's thread fiber；Will hydrolysis nylon 6 fiber and water in mass ratio 10：1
Mixing is added in three-necked flask, and the mass fraction for sequentially adding 0.4~0.6 times of hydrolysis nylon 6 fiber quality is molten for 90% phosphoric acid
Liquid, the mass fraction of 0.3~0.5 times of hydrolysis nylon 6 fiber quality is 20~40% organic acid solns, and three-necked flask is moved into number
Aobvious constant temperature blender with magnetic force, nitrogen is passed through into three-necked flask with 8~15mL/min speed, is 110~120 DEG C in temperature, is turned
Speed is 300~400r/min, under the conditions of pressure is 0.06~0.08MPa, after depressurizing 1~2h of constant temperature stirring reaction, then to three mouthfuls
Flask adds the degraded spider's thread fiber of 0.4~0.6 times of hydrolysis nylon 6 fiber quality, and is 260~300 DEG C in temperature, and rotating speed is
300~400r/min, under the conditions of pressure is 0.06~0.08MPa, after depressurizing 6~8h of constant temperature stirring reaction, standing is cooled to room
Temperature, mixed liquor is filtered, obtain No. 2 filter cakes；By organosilicon and ether in mass ratio 1：30 mixing are added in beaker, are stirred with glass bar
10~20min of dissolving is mixed, obtains organosilicon diethyl ether solution, and No. 2 filter cakes of 0.5~0.7 times of organosilicon diethyl ether solution quality are soaked
Stain in beaker, and into beaker add No. 2 0.1~0.3 times of filter cake qualities catalyst, in temperature be 35~40 DEG C, rotating speed
Under conditions of 400~600r/min, constant temperature 50~60min of stirring reaction, question response terminates, and beaker is stood into 30~45min,
Filtering, obtains No. 3 filter cakes, by No. 3 filter cake vacuum freeze dryings, produces the fiber of modification of nylon 6.Described salting liquid is mass fraction
Any one in the lithium rhodanate solution that lithium-bromide solution or mass fraction for 85% are 85%.Described organic acid soln is
Any one in the acetum that the ethanedioic acid solution or mass fraction that mass fraction is 20~40% are 20~40%.Described
Organosilicon is any one in benzyl silane or diphenyl silane.Described catalyst is anhydrous magnesium sulfate or anhydrous slufuric acid
Any one in calcium.
Example 1
First by nylon 6 fiber and water in mass ratio 1：50 add stainless steel cauldrons in, in temperature be 300 DEG C, pressure 10MPa
Under conditions of, filtered after constant temperature and pressure reaction 15min, obtain No. 1 filtrate, rotation is transferred to by No. 1 filtrate, and by No. 1 filtrate of gained
Evaporimeter, it is 50 DEG C in temperature, under the conditions of pressure is 800Pa, vacuum rotary steam concentration 6h, obtains concentrate, concentrate vacuum is cold
It is lyophilized dry, obtain hydrolysis nylon 6 fiber；By the salting liquid in mass ratio 2 that spider's thread fiber and mass fraction are 85%：5 are put into beaker
In, beaker is moved into digital display temperature constant magnetic stirring instrument, is 40 DEG C in temperature, under conditions of rotating speed is 500r/min, constant temperature stirs
Reaction 60min is mixed, under stirring, the water of 20 times of salting liquid quality is added into beaker, continues constant temperature and is stirred
After 15min, beaker is stood into 2h, filter, obtain No. 1 filter cake, by No. 1 filter cake be put into vacuum it is dry and cold freeze it is dry, must degrade spider's thread fiber；
Will hydrolysis nylon 6 fiber and water in mass ratio 10：1 mixing is added in three-necked flask, sequentially adds hydrolysis nylon 6 fiber quality
0.6 times of mass fraction is 90% phosphoric acid solution, and the mass fraction of 0.5 times of hydrolysis nylon 6 fiber quality is 40% organic acid soln,
Three-necked flask is moved into digital display constant temperature blender with magnetic force, nitrogen is passed through into three-necked flask with 15mL/min speed, is in temperature
120 DEG C, rotating speed 400r/min, under the conditions of pressure is 0.08MPa, after depressurizing constant temperature stirring reaction 2h, then add to three-necked flask
Enter to hydrolyze the degraded spider's thread fiber of 0.6 times of nylon 6 fiber quality, and be 300 DEG C, rotating speed 400r/min in temperature, pressure is
Under the conditions of 0.08MPa, after depressurizing constant temperature stirring reaction 8h, standing is cooled to room temperature, and mixed liquor is filtered, obtains No. 2 filter cakes；To have
Machine silicon and ether in mass ratio 1：30 mixing are added in beaker, with glass bar stirring and dissolving 20min, obtain organosilicon diethyl ether solution,
And No. 2 filter cakes of 0.7 times of organosilicon diethyl ether solution quality are impregnated in beaker, and No. 2 filter cake qualities 0.3 are added into beaker
Catalyst again, it is 40 DEG C in temperature, under conditions of rotating speed is 600r/min, constant temperature stirring reaction 60min, question response terminates,
Beaker is stood into 45min, is filtered, is obtained No. 3 filter cakes, by No. 3 filter cake vacuum freeze dryings, produce the fiber of modification of nylon 6.Described
Salting liquid is the lithium-bromide solution that mass fraction is 85%.Described organic acid soln is that the ethanedioic acid that mass fraction is 40% is molten
Liquid.Described organosilicon is benzyl silane.Described catalyst is anhydrous magnesium sulfate.
Example 2
First by nylon 6 fiber and water in mass ratio 1：50 add stainless steel cauldrons in, in temperature be 300 DEG C, pressure 10MPa
Under conditions of, filtered after constant temperature and pressure reaction 15min, obtain No. 1 filtrate, rotation is transferred to by No. 1 filtrate, and by No. 1 filtrate of gained
Evaporimeter, it is 50 DEG C in temperature, under the conditions of pressure is 800Pa, vacuum rotary steam concentration 6h, obtains concentrate, concentrate vacuum is cold
It is lyophilized dry, obtain hydrolysis nylon 6 fiber；Will hydrolysis nylon 6 fiber and water in mass ratio 10：1 mixing is added in three-necked flask, then according to
The secondary mass fraction for adding 0.6 times of hydrolysis nylon 6 fiber quality is 90% phosphoric acid solution, 0.5 times of hydrolysis nylon 6 fiber quality
Mass fraction is 40% organic acid soln, three-necked flask is moved into digital display constant temperature blender with magnetic force, with 15mL/min speed to three mouthfuls
Nitrogen is passed through in flask, is 120 DEG C, rotating speed 400r/min in temperature, under the conditions of pressure is 0.08MPa, decompression constant temperature stirs
After reacting 2h, standing is cooled to room temperature, and mixed liquor is filtered, obtains No. 2 filter cakes；By organosilicon and ether in mass ratio 1：30 mixing
Add in beaker, with glass bar stirring and dissolving 20min, obtain organosilicon diethyl ether solution, and by 0.7 times of organosilicon diethyl ether solution quality
No. 2 filter cakes be impregnated in beaker, and into beaker add No. 2 0.3 times of filter cake qualities catalyst, in temperature be 40 DEG C, turn
Under conditions of speed is 600r/min, constant temperature stirring reaction 60min, question response terminates, and beaker is stood into 45min, filtering, obtains No. 3
Filter cake, by No. 3 filter cake vacuum freeze dryings, produce the fiber of modification of nylon 6.Described salting liquid is the bromine that mass fraction is 85%
Change lithium solution.Described organic acid soln is the ethanedioic acid solution that mass fraction is 40%.Described organosilicon is benzyl silicon
Alkane.Described catalyst is anhydrous magnesium sulfate.
Example 3
First by nylon 6 fiber and water in mass ratio 1：50 add stainless steel cauldrons in, in temperature be 300 DEG C, pressure 10MPa
Under conditions of, filtered after constant temperature and pressure reaction 15min, obtain No. 1 filtrate, rotation is transferred to by No. 1 filtrate, and by No. 1 filtrate of gained
Evaporimeter, it is 50 DEG C in temperature, under the conditions of pressure is 800Pa, vacuum rotary steam concentration 6h, obtains concentrate, concentrate vacuum is cold
It is lyophilized dry, obtain hydrolysis nylon 6 fiber；By the salting liquid in mass ratio 2 that spider's thread fiber and mass fraction are 85%：5 are put into beaker
In, beaker is moved into digital display temperature constant magnetic stirring instrument, is 40 DEG C in temperature, under conditions of rotating speed is 500r/min, constant temperature stirs
Reaction 60min is mixed, under stirring, the water of 20 times of salting liquid quality is added into beaker, continues constant temperature and is stirred
After 15min, beaker is stood into 2h, filter, obtain No. 1 filter cake, by No. 1 filter cake be put into vacuum it is dry and cold freeze it is dry, must degrade spider's thread fiber；
Will hydrolysis nylon 6 fiber and water in mass ratio 10：1 mixing is added in three-necked flask, sequentially adds hydrolysis nylon 6 fiber quality
0.6 times of mass fraction is 90% phosphoric acid solution, and the mass fraction of 0.5 times of hydrolysis nylon 6 fiber quality is 40% organic acid soln,
Three-necked flask is moved into digital display constant temperature blender with magnetic force, nitrogen is passed through into three-necked flask with 15mL/min speed, is in temperature
120 DEG C, rotating speed 400r/min, under the conditions of pressure is 0.08MPa, after depressurizing constant temperature stirring reaction 2h, then add to three-necked flask
Enter to hydrolyze the degraded spider's thread fiber of 0.6 times of nylon 6 fiber quality, and be 300 DEG C, rotating speed 400r/min in temperature, pressure is
Under the conditions of 0.08MPa, after depressurizing constant temperature stirring reaction 8h, standing is cooled to room temperature, and mixed liquor is filtered, No. 2 filter cakes are obtained, by 2
Number filter cake vacuum freeze drying, produces the fiber of modification of nylon 6.Described salting liquid is the lithium-bromide solution that mass fraction is 85%.
Described organic acid soln is the ethanedioic acid solution that mass fraction is 40%.
Comparative example：The nylon 6 fiber of Suzhou plasticizing Co., Ltd production.
The fiber of modification of nylon 6 of the gained of example 1 to 3 and comparative example product are subjected to performance detection, specific detection method is such as
Under：
1. friction stability：Friction-wear test is carried out on UMT-3 frictional testing machines, and test parameters is as follows：Load 100N, turn
Fast 200r/min, time 120min, dry friction slide, mating plate be 9.5mm chromium steel ball, hardness HRC62.Specimen size 25mm
× 25mm × 10mm, sample surfaces are smooth with 1000 mesh liquid honings before experiment, and clean sample and antithesis surface with acetone.
Speed, time, load are definite value, and whole experiment is automatically performed by the program finished in advance to control, and test data is by computer
Automatic data collection, average friction coefficient are calculated into the test data for stablizing friction phase by material and are averagely worth to；
2. tensile property：Tested by GB/T1040, sample size is 150mm × 10mm × 4mm, draw speed 50mm/min；
3. bending property：Tested by GB/T9341, bending sample size is 100mm × 15mm × 10mm, speed 2mm/min；
4. notch impact strength：Tested by GB/T1043.1, specimen size is 80mm × 10mm × 4mm.
Specific testing result is as shown in table 1：
Table 1
From the testing result of table 1, the fiber of modification of nylon 6 prepared by technical solution of the present invention has excellent friction stability,
The characteristics of notch impact strength is high, and toughness is strong, has broad prospects in the development of spinning material field industry.
Claims (5)
1. a kind of preparation method of the fiber of modification of nylon 6, it is characterised in that specifically preparation process is：
（1）By nylon 6 fiber and water in mass ratio 1：50 mixing, constant temperature and pressure react 10~15min, filter, and dry, must hydrolyze
Nylon 6 fiber；
（2）By spider's thread fiber and salting liquid in mass ratio 2：5 are put into beaker, mix 40~60min, add salting liquid
The water that 15~20 times of quality, filtered after being uniformly mixed, filtrate is concentrated, dried, must degrade spider's thread fiber；
（3）Will hydrolysis nylon 6 fiber and water in mass ratio 10：1 mixing, sequentially add hydrolysis nylon 6 fiber quality 0.4~
0.6 times of phosphoric acid solution, the organic acid soln of 0.3~0.5 times of hydrolysis nylon 6 fiber quality, under the protection of nitrogen, decompression is permanent
Warm stirring reaction, then heat up, and the degraded spider's thread fiber of 0.4~0.6 times of hydrolysis nylon 6 fiber quality is added, it is permanent to continue constant temperature
Pressure 6~8h of reaction, cools down, filtering, obtains filter cake；
（4）By organosilicon and ether in mass ratio 1：30 mixing, obtain organosilicon diethyl ether solution, filter cake are impregnated in into organosilicon ether
In solution, the catalyst of 0.1~0.3 times of filter cake quality is added, after 50~60min of stirring reaction, stand, filtering, vacuum is done
It is dry, produce the fiber of modification of nylon 6.
A kind of 2. preparation method of the fiber of modification of nylon 6 according to claim 1, it is characterised in that：Step（2）Described
Any one in the lithium rhodanate solution that salting liquid is the lithium-bromide solution that mass fraction is 85% or mass fraction is 85%.
A kind of 3. preparation method of the fiber of modification of nylon 6 according to claim 1, it is characterised in that：Step（3）Described
Organic acid soln is appointing in the acetum that the ethanedioic acid solution that mass fraction is 20~40% or mass fraction are 20~40%
Meaning is a kind of.
A kind of 4. preparation method of the fiber of modification of nylon 6 according to claim 1, it is characterised in that：Step（4）Described
Organosilicon is any one in benzyl silane or diphenyl silane.
A kind of 5. preparation method of the fiber of modification of nylon 6 according to claim 1, it is characterised in that：Step（4）Described
Catalyst is any one in anhydrous magnesium sulfate or dead plaster.
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