CN109321999A - A kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon and preparation method thereof - Google Patents
A kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon and preparation method thereof Download PDFInfo
- Publication number
- CN109321999A CN109321999A CN201811206953.8A CN201811206953A CN109321999A CN 109321999 A CN109321999 A CN 109321999A CN 201811206953 A CN201811206953 A CN 201811206953A CN 109321999 A CN109321999 A CN 109321999A
- Authority
- CN
- China
- Prior art keywords
- reaction
- caprolactam
- volcanic rock
- temperature
- spinning
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
-
- 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
- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention relates to a kind of efficient far infrareds, 6 fiber of ultraviolet resistant nylon and preparation method thereof, using situ aggregation method, in caprolactam ring-opening polymerisation, volcanic rock and butyl titanate are dispersed in caprolactam water solution, caprolactam polymerization reaction generating portion water, promote butyl titanate in-situ hydrolysis, nano-titanium dioxide and uniform adsorption are generated on volcanic rock surface, butyl titanate can promote volcanic rock and be dispersed in caprolactam water solution simultaneously, then polymerization obtains high dispersancy nano volcanic rock/nano-titanium dioxide modified nylon 6, 6 composite fibre of ultraviolet resistant nylon is obtained finally by melt spinning.Program synthesis technology is simple, it is at low cost, solve the problems, such as that current titanium dioxide disperses unevenness in 6 melt of nylon, the characteristics such as nylon 6 fiber uvioresistant, far infrared, warming are assigned simultaneously, product is soft, uvioresistant performance is lasting, can undergo multiple washing, can be widely used in home textile, takes, the fields such as sports and leisure.
Description
Technical field
The present invention relates to a kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon, specifically a kind of high dispersancy nano fire
Mountain rock/6 composite fibre of nano-titanium dioxide/nylon and preparation method thereof, belongs to the manufacturing technology field of chemical fibre.
Background technique
Nylon fibre be realize earliest in the world had excellent performance in industrialized synthetic fibers and synthetic fibers, purposes
One of extensive kind, it has many excellent performances, goes rotten in addition to having shared corrosion-resistant, resistance to of synthetic fibers, is wet strong
Degree is high, is not afraid of and damages by worms, outside the performances such as hydroscopicity is low, also has that intensity is high, wearability is excellent, elasticity is good, elongate fiber response rate
The advantages that high.With people's improvement of living standard, people are to comfortable, the healthcare function growing interest of textile, to the more of fiber
Functionalization requirement is more more and more intense, and research, exploitation and the production of the various differential nylon fibres of functionalization are paid more attention to.
Health perception is improved recently as people, obtains people's by depletion of the ozone layer bring ultraviolet radioactive problem
Extensive concern.Ultraviolet light can classify according to wavelength difference: long wave ultraviolet UVA (320~400nm), ultraviolet B radiation UVB
(280~320nm) and short wave ultraviolet UVC (< 280nm).Excessive ultraviolet radiation can accelerate skin aging or even carcinogenic.Cause
This clothes and raw material with uvioresistant safeguard function attract wide public concern.Recently as being constantly progressive for nanosecond science and technology,
The preparation and application of nano-titanium dioxide have obtained extensive attention, especially rutile titanium dioxide and have absorbed purple due to having
Excellent optical property, the nano silicas such as outer light, higher refractive index (2.6-2.9) can be used as excellent uvioresistant
Agent, which is widely used in spinning, takes field.
Currently, the method for preparing ultraviolet resistant nylon 6 mainly has final finishing cladding process, physical blending process and in-situ copolymerization method
Deng.It focused mostly on about the method for preparing antiultraviolet fiber in final finishing cladding process, although being easy to be mass produced, knitted in recent years
Object feel is harder, and durability is poor；And blend modification technology is before spinning, directly to add nanoparticle under mechanical force
Enter and mixed into polymeric matrix, including melt-blending process and solution blended process etc., blending method is easy to operate, it is easy to accomplish
Industrialization, but nanoparticle is easily reunited, and is difficult to be uniformly dispersed in a polymer matrix.In-situ copolymerization method is in nylon polymerization
Before, nano-powder is distributed in monomer, then a kind of method being polymerize, this method is easy to operate, low in cost, environmental protection section
Can, while it can be also obviously improved nano-powder agglomeration, it is more and more concerned at present.
It is mainly real that nanometer volcanic rock/nano-titanium dioxide/nylon 6 composite material difficult point of function admirable, which is prepared,
Evenly dispersed, titanium dioxide high crystalline, the replacement cycle that extends filament spinning component, raising of the existing function powder in nylon melt
The machinability etc. of functional fibre.Chinese invention patent " a kind of ultraviolet aging resistance fire-retardant nylon composite material and preparation method "
(CN107446349A) in, nylon chips, fire retardant, age resister, glass fibre etc. is uniformly mixed, twin-screw extrusion is passed through
Machine melt blending extruding pelletization, obtains resistance to ultraviolet aging-resistant flame-proof nylon composite materials, but its bad dispersibility, needs to be added each
Kind auxiliary agent, it is at high cost.A kind of Chinese invention patent " nano-titanium dioxide nylon 66 resin prepared with anti-ultraviolet function
With the method for fiber " in (CN104629042A), it is molten to polymer at flash distillation pump discharge in nylon66 fiber polycondensation process
TiO is injected in body2Suspension, thus by TiO2It is dispersed in nylon66 fiber, but its dispersibility is not improved.In
In state's patent of invention " a kind of ultraviolet ray resistant textiles " (CN104695225A), describes and increased by padding fluorescence to nylon textile
White dose, improve the uvioresistant performance of textile.But technique high production cost, not environmentally, fabric are harder and intolerant to washing.
To solve the above problems, the present invention uses situ aggregation method, in caprolactam ring-opening polymerisation, by volcanic rock and titanium
Sour four butyl esters are dispersed in caprolactam water solution, and caprolactam polymerization reaction generating portion water promotes butyl titanate
In-situ hydrolysis, generates nano-titanium dioxide and uniform adsorption is on volcanic rock surface, while butyl titanate promotes volcanic rock uniform
It is dispersed in caprolactam water solution, then polymerization obtains polymolecularity volcanic rock/titania modified nylon 6, finally by
Melt spinning obtains 6 composite fibre of ultraviolet resistant nylon.The nano-titanium dioxide that butyl titanate in-situ hydrolysis generates uniformly is born
It is loaded in volcanic rock surface, can dramatically improve dispersibility of the nano-titanium dioxide in caprolactam, while four fourth of metatitanic acid
It is evenly dispersed that ester also can promote nanometer volcanic rock.By deploying the ratio of water and caprolactam, in-situ hydrolysis temperature, four fourth of metatitanic acid
Ester concentration, the techniques such as nanometer volcanic rock concentration, it can be achieved that nano-titanium dioxide and nanometer volcanic rock in the big of caprolactam content
Range.The present invention solves the problems, such as current nano-titanium dioxide difficulties in dispersion in nylon matrix, simple process, and normal
It is almost the same to advise polymerization technique, and greatly remains the performance of each component, at the same impart the excellent far infrared of nylon 6 fiber,
Uvioresistant performance.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of efficient far infrareds, 6 fiber of ultraviolet resistant nylon
Preparation method, volcanic rock and butyl titanate are dispersed in caprolactam ring-opening polymerisation using situ aggregation method
In caprolactam water solution, caprolactam polymerization reaction generating portion water promotes butyl titanate in-situ hydrolysis, generates nanometer two
Titanium oxide and uniform adsorption are on volcanic rock surface, while butyl titanate promotes volcanic rock to be dispersed in caprolactam water solution
In, then polymerization obtains polymolecularity volcanic rock/titania modified nylon 6, obtains uvioresistant Buddhist nun finally by melt spinning
Imperial 6 composite fibres.Program synthesis technology is simple, at low cost, solves current titanium dioxide and disperses unevenness in 6 melt of nylon
The problem of, while the characteristics such as nylon 6 fiber far infrared, uvioresistant are assigned, and do not influence nylon 6/poly conjunction, to guarantee that nylon 6 has
There are good fibre forming property and the excellent quality of fiber, and product is soft, far infrared, uvioresistant performance are lasting, can undergo
Repeatedly washing.A kind of prepared efficient far infrared, 6 fiber of ultraviolet resistant nylon can be widely used in home textile, take, sports and leisure
Equal fields.
To reach above-mentioned technical purpose, the invention adopts the following technical scheme:
(1) nanometer volcanic rock and butyl titanate are placed in caprolactam water solution, it is raw by butyl titanate in-situ hydrolysis
At nano-titanium dioxide and uniform adsorption is on volcanic rock surface, while butyl titanate promotes nanometer volcanic rock to be dispersed in again
It is formed in caprolactam water solution and stablizes volcanic rock/titanium dioxide/caprolactam water solution.Contain in the caprolactam water solution
Caprolactam is 10-90wt%, is formed by nanometer volcanic rock content in volcanic rock/titanium dioxide/caprolactam water solution and accounts for oneself
The 0.1-10wt% of lactam content, nanometer titanium dioxide Ti content account for the 0.01-10wt% of caprolactam content, the hydrolysis temperature
It is 80-140 DEG C.
(2) (1) obtained slurries and additive are placed in pressure is to carry out ring-opening reaction under 0.3-5MPa pressure, in this mistake
Cheng Zhong, reaction temperature are 220-300 DEG C, reaction time 1-6h, and key reaction is the hydrolysis of caprolactam, and addition is anti-
The water answered, while generated in system promotes unreacted butyl titanate in-situ hydrolysis to generate nano-titanium dioxide uniform adsorption again
On nanometer volcanic rock surface；The additive is one or more of adipic acid, acetic acid, terephthalic acid (TPA), and additive amount is opposite
In the 0.01-1wt% of quality of caprolactam.
(3) (2) obtained melt is placed under normal pressure to the reaction was continued.Reaction temperature is 220-280 DEG C, reaction time 3-
8h.Polycondensation reaction of this process key reaction between 6 oligomer of nylon.
(4) according to the requirement of final products, (3) obtained melt is placed under vacuum environment and is reacted, pressure 0-
200pa, reaction temperature are 220-280 DEG C, reaction time 0-3h, this reaction is mainly that the amide exchange of 6 strand of nylon is anti-
Answer and remove the process of small molecule.
(5) it by obtained melt in (4) after cooling, pelletizing, extraction, drying, then send to spinning threadling and carries out melt spinning, obtain
Obtain far infrared, 6 fiber of ultraviolet resistant nylon.
Main chemical reactions equation are as follows:
(1) ring-opening reaction
(2) graft reaction
(3) addition reaction
(4) polycondensation reaction
(5) amide exchange reaction
(6) in-situ hydrolysis reacts
。
The spinning process of as described above efficiently far infrared, 6 fiber of ultraviolet resistant nylon, the technique of melt spinning specifically:
The FDY technique specifically:
Spinning temperature is 240-280 DEG C, and the first draw-off godet speed is 4000-4500m/min, and second spinning reel speed is 5000-
6000m/min, draw ratio are 1.1-1.5 times, and cooling wind temperature is 15-25 DEG C, wind speed 0.5-1m/s, relative humidity 60%-
90%, obtain fully drawn yarn；
The UDY technique specifically:
Spinning temperature is 240-280 DEG C, spinning speed 700-1500m/min, and cooling wind temperature is 20-30 DEG C, wind speed 0.3-1m/
S, relative humidity 60%-80% obtain non-oriented silk；
The POY technique specifically:
Spinning temperature is 240-280 DEG C, spinning speed 4000-4500m/min, and cooling wind temperature is 15-25 DEG C, wind speed 0.3-
0.6m/s, relative humidity 60%-80%, obtains preoriented yarn；
The HOY technique specifically:
Spinning temperature is 240-280 DEG C, spinning speed 4500-6000m/min, and cooling wind temperature is 15-20 DEG C, wind speed 0.3-
0.5m/s, relative humidity 80%-90%, obtains high oriented yarn；
The BCF technique specifically:
Spinning temperature is 240-280 DEG C, and cooling wind temperature is 20-30 DEG C, wind speed 0.3-1m/s, relative humidity 60%-80%, feeding
Roll temperature is 60-120 DEG C, and draw roll temperature is 100-190 DEG C, feeding speed 300-1000m/min, and tensile speed is
1000-3500m/min, draw ratio are 3.5-5 times, and deformation hot air temperature is 190-230 DEG C, and air injection pressure is
196kPa-490kPa, winding speed 600-3000m/min, cooling air temperature are 25 DEG C.
Beneficial effect.
1) in-situ hydrolysis method is used, tetrabutyl titanate hydrolysis is generated into nano-titanium dioxide simultaneously in caprolactam water solution
Uniform adsorption is on porosity nanometer volcanic rock, and butyl titanate can promote to improve nanometer volcanic rock in caprolactam
Dispersibility, the two mutually promotes, to further improve dispersibility of the nano-titanium dioxide in nylon 6, improves and receive
The utilization efficiency of rice titanium dioxide.
2) method for using in-situ polymerization, further improves nanometer volcanic rock and nano-titanium dioxide in nylon 6
Dispersion effect, to improve spinnability.
3) preparation-obtained nanometer volcanic rock/6 composite fibre of nano-titanium dioxide/nylon has uvioresistant, keeps warm, is remote red
The functions such as outer, can take, the fields such as home textile, carpet are applied.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
Embodiment 1.
A kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon spinning process be divided into following steps:
(1) nanometer volcanic rock and butyl titanate are placed in caprolactam water solution, it is raw by butyl titanate in-situ hydrolysis
At nano-titanium dioxide and uniform adsorption is on volcanic rock surface, while butyl titanate promotes nanometer volcanic rock to be dispersed in again
It is formed in caprolactam water solution and stablizes volcanic rock/titanium dioxide/caprolactam water solution.Contain in the caprolactam water solution
Caprolactam is 10wt%, is formed by nanometer volcanic rock content in volcanic rock/titanium dioxide/caprolactam water solution and accounts in oneself
The 0.1wt% of amide content, nanometer titanium dioxide Ti content account for the 0.01wt% of caprolactam content, and the hydrolysis temperature is 80 DEG C.
(2) (1) obtained slurries and additive are placed in pressure is to carry out ring-opening reaction under 0.3MPa pressure, in this process
In, reaction temperature is 220 DEG C, reaction time 1h, and key reaction is the hydrolysis of caprolactam, addition reaction, while body
The water generated in system promotes unreacted butyl titanate in-situ hydrolysis to generate nano-titanium dioxide uniform adsorption in nanometer fire again
The surface Shan Yan；The additive is adipic acid, and additive amount is the 0.01wt% relative to quality of caprolactam.
(3) (2) obtained melt is placed under normal pressure to the reaction was continued.Reaction temperature is 220 DEG C, reaction time 3h.This mistake
Polycondensation reaction of the journey key reaction between 6 oligomer of nylon.
(4) according to the requirement of final products, (3) obtained melt is placed under vacuum environment and is reacted, pressure 10pa,
Reaction temperature is 220 DEG C, reaction time 0.5h, this reaction is mainly the amide exchange reaction of 6 strand of nylon and removes small
The process of molecule.
(5) it by obtained melt in (4) after cooling, pelletizing, extraction, drying, then send to spinning threadling and carries out melt spinning, obtain
Obtain far infrared, 6 fiber of ultraviolet resistant nylon.
A kind of spinning process of graphene/nylon fiber as described above, the technique of the melt spinning specifically:
The FDY technique specifically:
Spinning temperature is 240 DEG C, and the first draw-off godet speed is 4000m/min, and second spinning reel speed is 5000m/min, is stretched
Multiple is 1.1 times, and cooling wind temperature is 15 DEG C, wind speed 0.5m/s, and relative humidity 60% obtains fully drawn yarn.
Embodiment 2.
A kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon spinning process be divided into following steps:
(1) nanometer volcanic rock and butyl titanate are placed in caprolactam water solution, it is raw by butyl titanate in-situ hydrolysis
At nano-titanium dioxide and uniform adsorption is on volcanic rock surface, while butyl titanate promotes nanometer volcanic rock to be dispersed in again
It is formed in caprolactam water solution and stablizes volcanic rock/titanium dioxide/caprolactam water solution.Contain in the caprolactam water solution
Caprolactam is 90wt%, is formed by nanometer volcanic rock content in volcanic rock/titanium dioxide/caprolactam water solution and accounts in oneself
The 10wt% of amide content, nanometer titanium dioxide Ti content account for the 10wt% of caprolactam content, and the hydrolysis temperature is 140 DEG C.
(2) (1) obtained slurries and additive are placed in pressure is to carry out ring-opening reaction under 5MPa pressure, in this process
In, reaction temperature is 300 DEG C, reaction time 6h, and key reaction is the hydrolysis of caprolactam, addition reaction, while body
The water generated in system promotes unreacted butyl titanate in-situ hydrolysis to generate nano-titanium dioxide uniform adsorption in nanometer fire again
The surface Shan Yan；The additive is acetic acid, and additive amount is the 1wt% relative to quality of caprolactam.
(3) (2) obtained melt is placed under normal pressure to the reaction was continued.Reaction temperature is 280 DEG C, reaction time 8h.This mistake
Polycondensation reaction of the journey key reaction between 6 oligomer of nylon.
(4) according to the requirement of final products, (3) obtained melt is placed under vacuum environment and is reacted, pressure is
200pa, reaction temperature are 280 DEG C, reaction time 3h, this reaction is mainly the amide exchange reaction of 6 strand of nylon and takes off
Except the process of small molecule.
(5) it by obtained melt in (4) after cooling, pelletizing, extraction, drying, then send to spinning threadling and carries out melt spinning, obtain
Obtain far infrared, 6 fiber of ultraviolet resistant nylon.
A kind of spinning process of graphene/nylon fiber as described above, the technique of the melt spinning specifically:
The POY technique specifically:
Spinning temperature is 280 DEG C, spinning speed 4500m/min, and cooling wind temperature is 25 DEG C, wind speed 0.6m/s, and relative humidity is
80%, obtain preoriented yarn.
Embodiment 3.
A kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon spinning process be divided into following steps:
(1) nanometer volcanic rock and butyl titanate are placed in caprolactam water solution, it is raw by butyl titanate in-situ hydrolysis
At nano-titanium dioxide and uniform adsorption is on volcanic rock surface, while butyl titanate promotes nanometer volcanic rock to be dispersed in again
It is formed in caprolactam water solution and stablizes volcanic rock/titanium dioxide/caprolactam water solution.Contain in the caprolactam water solution
Caprolactam is 50wt%, is formed by nanometer volcanic rock content in volcanic rock/titanium dioxide/caprolactam water solution and accounts in oneself
The 5wt% of amide content, nanometer titanium dioxide Ti content account for the 5wt% of caprolactam content, and the hydrolysis temperature is 90 DEG C.
(2) (1) obtained slurries and additive are placed in pressure is to carry out ring-opening reaction under 2.6MPa pressure, in this process
In, reaction temperature is 260 DEG C, reaction time 3.5h, hydrolysis of the key reaction for caprolactam, addition reaction, simultaneously
The water generated in system promotes unreacted butyl titanate in-situ hydrolysis to generate nano-titanium dioxide uniform adsorption in nanometer again
Volcanic rock surface；The additive is one or more of adipic acid, acetic acid, terephthalic acid (TPA), and additive amount is relative in oneself
The 0.5wt% of amide quality.
(3) (2) obtained melt is placed under normal pressure to the reaction was continued.Reaction temperature is 250 DEG C, reaction time 5.5h.This
Polycondensation reaction of the process key reaction between 6 oligomer of nylon.
(4) according to the requirement of final products, (3) obtained melt is placed under vacuum environment and is reacted, pressure 0-
200pa, reaction temperature be 250 DEG C, reaction time 1.5h, this reaction be mainly 6 strand of nylon amide exchange reaction and
Remove the process of small molecule.
(5) it by obtained melt in (4) after cooling, pelletizing, extraction, drying, then send to spinning threadling and carries out melt spinning, obtain
Obtain far infrared, 6 fiber of ultraviolet resistant nylon.
Claims (2)
1. the preparation method of a kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon, it is characterized in that: using situ aggregation method, in oneself
In amide ring-opening polymerisation, nanometer volcanic rock and butyl titanate are dispersed in caprolactam water solution, butyl titanate
In-situ hydrolysis generates nano-titanium dioxide and uniform adsorption on volcanic rock surface, with caprolactam polymerization reaction, the water of generation
Continue to promote butyl titanate in-situ hydrolysis, while butyl titanate promotes nanometer volcanic rock to be dispersed in caprolactam water again
In solution, continue polymerization and obtain polymolecularity volcanic rock/titania modified nylon 6, is obtained finally by melt spinning remote red
Outside, 6 fiber of ultraviolet resistant nylon；
Specific steps are as follows:
(1) nanometer volcanic rock and butyl titanate are placed in caprolactam water solution, it is raw by butyl titanate in-situ hydrolysis
At nano-titanium dioxide and uniform adsorption is on volcanic rock surface, while butyl titanate promotes nanometer volcanic rock to be dispersed in again
It is formed in caprolactam water solution and stablizes volcanic rock/titanium dioxide/caprolactam water solution, contained in the caprolactam water solution
Caprolactam is 10-90wt%, is formed by nanometer volcanic rock content in volcanic rock/titanium dioxide/caprolactam water solution and accounts for oneself
The 0.1-10wt% of lactam content, nanometer titanium dioxide Ti content account for the 0.01-10wt% of caprolactam content, the hydrolysis temperature
It is 80-140 DEG C；
(2) (1) obtained slurries and additive are placed in pressure is to carry out ring-opening reaction under 0.3-5MPa pressure, in this process
In, reaction temperature is 220-300 DEG C, reaction time 1-6h, hydrolysis of the key reaction for caprolactam, addition reaction,
The water generated in system simultaneously promotes unreacted butyl titanate in-situ hydrolysis generation nano-titanium dioxide uniform adsorption to exist again
Nanometer volcanic rock surface；The additive be one or more of adipic acid, acetic acid, terephthalic acid (TPA), additive amount be relative to
The 0.01-1wt% of quality of caprolactam；
(3) (2) obtained melt is placed under normal pressure to the reaction was continued, reaction temperature is 220-280 DEG C, reaction time 3-8h；
Polycondensation reaction of this process key reaction between 6 oligomer of nylon；
(4) according to the requirement of final products, (3) obtained melt is placed under vacuum environment and is reacted, pressure 0-200pa,
Reaction temperature is 220-280 DEG C, reaction time 0-3h, this reaction is mainly the amide exchange reaction of 6 strand of nylon and takes off
Except the process of small molecule；
(5) it by obtained melt in (4) after cooling, pelletizing, extraction, drying, then send to spinning threadling and carries out melt spinning, obtain remote
Infrared, 6 fiber of ultraviolet resistant nylon；
Main chemical reactions equation are as follows:
(1) ring-opening reaction
(2) graft reaction
(3) addition reaction
(4) polycondensation reaction
(5) amide exchange reaction
(6) in-situ hydrolysis reacts
。
2. a kind of efficient far infrared as claimed in claim 1, the preparation method of 6 fiber of ultraviolet resistant nylon, it is characterized in that:
The technique of the melt spinning specifically:
The FDY technique specifically:
Spinning temperature is 240-280 DEG C, and the first draw-off godet speed is 4000-4500m/min, and second spinning reel speed is 5000-
6000m/min, draw ratio are 1.1-1.5 times, and cooling wind temperature is 15-25 DEG C, wind speed 0.5-1m/s, relative humidity 60%-
90%, obtain fully drawn yarn；
The UDY technique specifically:
Spinning temperature is 240-280 DEG C, spinning speed 700-1500m/min, and cooling wind temperature is 20-30 DEG C, wind speed 0.3-1m/
S, relative humidity 60%-80% obtain non-oriented silk；
The POY technique specifically:
Spinning temperature is 240-280 DEG C, spinning speed 4000-4500m/min, and cooling wind temperature is 15-25 DEG C, wind speed 0.3-
0.6m/s, relative humidity 60%-80%, obtains preoriented yarn；
The HOY technique specifically:
Spinning temperature is 240-280 DEG C, spinning speed 4500-6000m/min, and cooling wind temperature is 15-20 DEG C, wind speed 0.3-
0.5m/s, relative humidity 80%-90%, obtains high oriented yarn；
The BCF technique specifically:
Spinning temperature is 240-280 DEG C, and cooling wind temperature is 20-30 DEG C, wind speed 0.3-1m/s, relative humidity 60%-80%, feeding
Roll temperature is 60-120 DEG C, and draw roll temperature is 100-190 DEG C, feeding speed 300-1000m/min, and tensile speed is
1000-3500m/min, draw ratio are 3.5-5 times, and deformation hot air temperature is 190-230 DEG C, and air injection pressure is
196kPa-490kPa, winding speed 600-3000m/min, cooling air temperature are 25 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811206953.8A CN109321999A (en) | 2018-10-17 | 2018-10-17 | A kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811206953.8A CN109321999A (en) | 2018-10-17 | 2018-10-17 | A kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109321999A true CN109321999A (en) | 2019-02-12 |
Family
ID=65262346
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811206953.8A Pending CN109321999A (en) | 2018-10-17 | 2018-10-17 | A kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109321999A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607836A (en) * | 2019-02-26 | 2020-09-01 | 南方寝饰科技有限公司 | Photocatalyst nylon fiber and preparation method and application thereof |
| CN115232302A (en) * | 2022-08-30 | 2022-10-25 | 杭州聚合顺新材料股份有限公司 | Method for simply and rapidly preparing nylon 66 nano composite material |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010051140A2 (en) * | 2008-10-08 | 2010-05-06 | Lilo Ben-Zicron | Friction material and method for making same |
| CN101768351A (en) * | 2008-12-29 | 2010-07-07 | 合肥杰事杰新材料有限公司 | Method for preparing mesoporous nano particle-enhanced nylon composite material |
| CN102409424A (en) * | 2011-12-13 | 2012-04-11 | 中原工学院 | Method for preparing bamboo charcoal and polyamide composite fibers by in situ polymerization |
| CN104480561A (en) * | 2014-12-12 | 2015-04-01 | 东华大学 | Caprolactam hydrolyzed polymer fibres and spinning method thereof |
| CN106947246A (en) * | 2017-05-08 | 2017-07-14 | 福建景丰科技有限公司 | A kind of fast thermal fiber of polyamide fibre 6 and its production method and the fast hot master batch of polyamide fibre 6 |
| CN107653507A (en) * | 2017-09-06 | 2018-02-02 | 广东大红马纺织新材料有限公司 | A kind of titania modified Fypro preparation method |
| CN107723828A (en) * | 2017-10-13 | 2018-02-23 | 江苏双良低碳产业技术研究院有限公司 | The preparation method and spinning process of a kind of polymolecularity graphene/composite fibre of nylon 6 |
-
2018
- 2018-10-17 CN CN201811206953.8A patent/CN109321999A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010051140A2 (en) * | 2008-10-08 | 2010-05-06 | Lilo Ben-Zicron | Friction material and method for making same |
| CN101768351A (en) * | 2008-12-29 | 2010-07-07 | 合肥杰事杰新材料有限公司 | Method for preparing mesoporous nano particle-enhanced nylon composite material |
| CN102409424A (en) * | 2011-12-13 | 2012-04-11 | 中原工学院 | Method for preparing bamboo charcoal and polyamide composite fibers by in situ polymerization |
| CN104480561A (en) * | 2014-12-12 | 2015-04-01 | 东华大学 | Caprolactam hydrolyzed polymer fibres and spinning method thereof |
| CN106947246A (en) * | 2017-05-08 | 2017-07-14 | 福建景丰科技有限公司 | A kind of fast thermal fiber of polyamide fibre 6 and its production method and the fast hot master batch of polyamide fibre 6 |
| CN107653507A (en) * | 2017-09-06 | 2018-02-02 | 广东大红马纺织新材料有限公司 | A kind of titania modified Fypro preparation method |
| CN107723828A (en) * | 2017-10-13 | 2018-02-23 | 江苏双良低碳产业技术研究院有限公司 | The preparation method and spinning process of a kind of polymolecularity graphene/composite fibre of nylon 6 |
Non-Patent Citations (1)
| Title |
|---|
| 何云鹏: "复合氧化物TiO2-SiO2的制备及其应用研究进展", 《精细石油化工进展》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607836A (en) * | 2019-02-26 | 2020-09-01 | 南方寝饰科技有限公司 | Photocatalyst nylon fiber and preparation method and application thereof |
| CN111607836B (en) * | 2019-02-26 | 2022-11-01 | 南方寝饰科技有限公司 | Photocatalyst nylon fiber and preparation method and application thereof |
| CN115232302A (en) * | 2022-08-30 | 2022-10-25 | 杭州聚合顺新材料股份有限公司 | Method for simply and rapidly preparing nylon 66 nano composite material |
| CN115232302B (en) * | 2022-08-30 | 2024-01-05 | 杭州聚合顺新材料股份有限公司 | Method for simply, conveniently and rapidly preparing nylon 66 nanocomposite |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107385545B (en) | A kind of preparation method and application of the copolyesteramide and its fiber that graphene oxide is modified | |
| CN106906535B (en) | A kind of graphene/nylon 6 fabric and preparation method thereof with permanent far-infrared health care function | |
| WO2018161766A1 (en) | Graphene/nylon-6 fiber, fabric and preparation method | |
| WO2019000985A1 (en) | Graphene composite material and preparation method therefor | |
| CN106350932B (en) | Flocking lace fabric | |
| CN107723828A (en) | The preparation method and spinning process of a kind of polymolecularity graphene/composite fibre of nylon 6 | |
| CN105063796A (en) | High-molecular composite conductive fiber and preparation method thereof | |
| CN105002595A (en) | Polymer composite function fibers containing partial graphene, and preparation method thereof | |
| CN101857981B (en) | Process for producing nanometer bamboo carbon fiber by adopting polylactic acid group | |
| CN101545154B (en) | Anion polyester fiber capable of being dyed at normal temperature and normal pressure, preparation method and application thereof | |
| JP7053956B2 (en) | Wool-like polyester filament and its manufacturing method | |
| CN107779984B (en) | Nano-material modified PBT spinning | |
| CN108221078A (en) | A kind of manufacturing method of polyester filament | |
| CN106350883A (en) | Preparation method of graphene oxide/polyacrylonitrile composite fiber | |
| CN109321999A (en) | A kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon and preparation method thereof | |
| CN105177751A (en) | Colored anti-ultraviolet profiled fine denier polyester filament and preparation method thereof | |
| CN111910285A (en) | Graphene biological composite fiber and preparation method and application thereof | |
| CN110714236A (en) | Preparation method of moisture-absorbing sweat-releasing antibacterial polyester filament yarn | |
| WO2020006693A1 (en) | Application of profiled fiber in infrared radiation material and textile | |
| CN105887231B (en) | A kind of manufacture method of fused mass directly spinning high strength polyester filament yarn | |
| CN110670167A (en) | Preparation method of antibacterial polyester staple fibers | |
| CN103556465A (en) | Method for compounding natural protein fiber powder on surfaces of polymer filaments | |
| CN109440223A (en) | A kind of wet fiber material preparation method of spiral porous structure | |
| CN111733477A (en) | High-performance nano ceramic uvioresistant high-cold-insulation fiber and preparation method thereof | |
| CN1552765A (en) | Method for preparing uvioresistant polyester by nanometer titania generated in situ |
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 | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190212 |