CN106835313A - A kind of nano-zirconium carbide of organic modification and its application in polyamide fibre preparation - Google Patents
A kind of nano-zirconium carbide of organic modification and its application in polyamide fibre preparation Download PDFInfo
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- CN106835313A CN106835313A CN201611057890.5A CN201611057890A CN106835313A CN 106835313 A CN106835313 A CN 106835313A CN 201611057890 A CN201611057890 A CN 201611057890A CN 106835313 A CN106835313 A CN 106835313A
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- zirconium carbide
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- polyamide fibre
- polycaprolactam
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/10—Metal compounds
- C08K3/14—Carbides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides a kind of method for organic modification of nano-zirconium carbide, and extinction containing the modified Nano zirconium carbide generates heat the preparation method of polyamide fibre.The present invention is processed nano-zirconium carbide using trimethoxy chlorosilane, trimethoxy chlorosilane is set to be reacted with zirconium carbide surface hydroxyl, obtain the organic modification nano-zirconium carbide of Surface coating trimethoxy silicon, then modified Nano zirconium carbide is added into fibre polycaprolactam and is made functional agglomerate, functional agglomerate is mixed with polycaprolactam section again, extinction heating polyamide fibre is obtained through melting, spinning, stretching, winding.The content of modified Nano zirconium carbide is 10~15wt% in master batch, and master batch is 20/80~10/90 with the blending ratio (mass ratio) of section, and the content of modified Nano zirconium carbide is 1.0~3.1% in fiber.Polyamide fibre, good spinnability are prepared using the method, product has good extinction heating function and physical and mechanical properties.
Description
Technical field
The present invention relates to a kind of method for organic modification of nano-zirconium carbide, and the suction containing the modified Nano zirconium carbide
The preparation method of light heating polyamide fibre, belongs to functional fibre material technical field.
Background technology
It is one of topmost function of clothes that resisting cold is warming.Conventional garment material is mainly by controlling human body and external environment
Between heat transfer, thermal convection current and heat radiation and play resisting cold thermal effect.Normal body temperature is less than in ambient temperature
When, the heat exchange between human body and external environment can be reduced by the appropriate thickness for increasing clothing, so as to maintain human body
Normal body temperature.Increasingly raising with people to fashion and aesthetic, lightening to have become trend, especially winter
Sportswear, abundant too fat to move clothes not only influence attractive in appearance, have an effect on its sporting functionality.In order to improve the insulation of textile material
Effect, Japanese Zhong Fang companies, Kuraray company, mitsubishi rayon and Tianjin University of Technology etc. are by polyester, polyamides
The ceramic with high radiant rate far infrared is mixed into amine, polypropylene or polyacrylonitrile, far infrared heating fiber is prepared for.
The fabric being made of this fiber, with preferable heat insulation effect, but still it was not only slim and graceful but also warming to meet water clothes
It is required that.Then, having research and development person to be devoted to again can be from the exploitation of the heat generating fiber of outside energy absorption.For example, being led using micro-
" Dong Lire " fiber that electric material generates heat after being powered, and the change generated heat by the dioxygen oxidation in air using materials such as iron powders
Learn reaction heat generating fiber etc..But, the fabric and clothes being made of this fiber but have dress to use inconvenience and poor durability
Shortcoming.
Extinction heat generating fiber refers to that can absorb the visible ray and near infrared ray in sunshine, light and various light sources, and will
It is converted into the fiber that heat energy is discharged.Group IV transition can belong to carbide or the oxidation of element in the periodic table of chemical element
Thing, such as zirconium carbide (ZrC), titanium oxide (TiO2) etc., the absorptivity to visible ray is high, by radianting capacity after illumination and heating effect
It is good.For example, Tai Sate companies of Japan and You Nijika companies in polyamide, polyester by adding ZrC and metallic aluminium powder, exploitation
The sunlight thermal storage fiber of the entitled Solar- α of viable commercial product, 8 DEG C of clothes Nei Wenduda can be significantly improved under sunlight irradiation.Specially
Sharp CN103132177A is prepared for monofilament fineness for 2- by the nanometer ZrC of the online addition 1-8wt% in polyester fiber
The extinction heat generating fiber of 5dtex.Because nano material specific surface area is big, surface can be high, easily reunites in polymeric matrix,
So as to cause, fiber spinnability is poor, properties of product decline, and spins fine count fiber difficult.In order to obtain fiber of good performance, it is necessary to
Make that nano-particle is uniform and stable to be dispersed in polymeric matrix, keep the nano-scale particle size of nano material.Patent
CN103436976A is by SiC, MgO, ZnO, Al2O3Deng the organic modification of nano-particle, nano-particle is improve in polyene
Uniform and stable dispersive property in alkyl body, has been obtained the enhanced polypropylene of mechanical property, polyethylene composite fibre.Patent
CN103484959A discloses a kind of zirconium carbide composition in fibrous material and preparation method thereof, and the composition includes
Zirconium carbide, metal oxide and resin, said composition can improve the concavo-convex and sharp outward appearance on Zirconium carbide powder surface, and its in fibre
Dispersion in dimension, is conducive to following process.
The content of the invention
One object of the present invention in order to solve nano-zirconium carbide in fiber-forming polymer, especially into fine polycaprolactam tree
Uniform and stable scattering problem in fat, and a kind of method for organic modification of the nano-zirconium carbide for proposing.
Another object of the present invention is that the modified Nano zirconium carbide for obtaining is applied to the preparation of polyamide fibre, to be had
There is the polyamide fibre material of extinction heat generation characteristic.
To achieve the above object, solution of the invention is：
The first step：By mass, in 100 parts of butyl oxides, it is the nano silicon carbide of 100-300nm to add 20~25 parts of particle diameters
Zirconium, grinding distribution 1h, is obtained nano-zirconium carbide dispersion liquid at room temperature；
Second step：Added in dispersion liquid obtained by the first step trimethoxy chlorosilane (consumption for nano-zirconium carbide 3~
5wt%), stirring is warming up to 40 DEG C, reacts 1h；
3rd step：By second step gained reaction solution, it is spray-dried, obtain the organic modification of Surface coating trimethoxy silicon
Nano-zirconium carbide.
X-ray photoelectron power spectrum (XPS) figure (referring to Fig. 1) of zirconium carbide show, the meeting in storing process due to zirconium carbide
Generation oxidation, hydrolysis, a number of-OH is contained on its surface.These-OH can replace with trimethoxy chlorosilane
Reaction, so as to the trimethoxy silicon group in the connection of zirconium carbide surface, its reaction mechanism mechanism of reaction is shown in accompanying drawing 2.
Obtained modified Nano zirconium carbide is blended with polycaprolactam, to be made polyamide fibre material, to obtain extinction hair
Thermal characteristics.The method for producing this kind of polyamide fibre material is as follows：
First by mass, by 12~18 parts of obtained organic modification nano-zirconium carbide with 100 parts into fibre polycaprolactam
Polyimide resin is blended, and through screw extruder melt blending extrusion, granulation, functional agglomerate is obtained；
Obtained functional agglomerate and polycaprolactam are cut into slices again is blended, be obtained through melting, spinning, stretching, winding and inhaled
Light heating polyamide fibre, functional agglomerate is cut into slices with polycaprolactam and be blended by 20/80~10/90 mass ratio.
Beneficial effect
(1) method for organic modification of nano-zirconium carbide provided by the present invention, preparation process is easy, it is easy to industrial metaplasia
Produce, organic coating layer in surface is complete, can be effectively improved uniform and stable dispersive property of the nano-zirconium carbide in polymeric matrix.
(2) preparation method of the extinction heating polyamide fibre containing the modified Nano zirconium carbide that organises provided by the present invention, can spin
Property is good, can prepare fine count fiber (monofilament fineness ＜ 1.0dtex), and product has good physical and mechanical properties, adds in less
Under dosage, you can obtain good extinction heating property.
Brief description of the drawings
Fig. 1 is x-ray photoelectron power spectrum (XPS) figure of zirconium carbide；
Fig. 2 is the course of reaction of the trimethoxy silicon group in the connection of zirconium carbide surface；
Fig. 3 is the extinction heating property test result that the polyamide fibre material containing zirconium carbide of the present invention has.
Specific embodiment
The present invention is conducted further description with reference to embodiment.
Embodiment 1
The first step：By mass, in 100 parts of butyl oxides, the nano-zirconium carbide that 20 parts of particle diameters are 100~300nm is added,
Using horizontal mill, grinding distribution 1h, is obtained nano-zirconium carbide dispersion liquid at room temperature；
Second step：Reactor will be moved into first step gained dispersion liquid, (consumption is nano-sized carbon to add trimethoxy chlorosilane
Change the 5wt% of zirconium), 40 DEG C are warming up under agitation, react 1h；
3rd step：Reaction solution obtained by second step, spray-dried machine are dried.Drying process be feed rate 3.0~
4.0kg/h, 180~190 DEG C of import air temperature, 90~100 DEG C of air temperature of outlet, 0.35~0.40m of air draft speed3/ min, mist
Change 100~120kPa of pressure；
4th step：By mass, 12 parts of organic modification nano-zirconium carbide obtained by the 3rd step is gathered in oneself with 100 parts
Amide resin is extruded through screw extruder melt blending, granulation, and functional agglomerate is obtained.Blending technology is screw speed 150rpm,
Each area's temperature is followed successively by 210 ± 3 DEG C, 250 ± 3 DEG C, 245 ± 3 DEG C, 235 ± 3 DEG C, 180 ± 3 DEG C.
5th step：By mass, 10 parts of functional agglomerate obtained by the 4th step is blended with 90 parts of polycaprolactams, warp
Melting, spinning, stretching, winding are obtained extinction heating nylon fibre, and its performance indications is referring to table 1.Spinning technique is screw speed
45r/min, each area's temperature of screw extruder is followed successively by 262 ± 3 DEG C, 266 ± 3 DEG C, 267 ± 3 DEG C, 270 ± 3 DEG C, 270 ± 3 DEG C,
Orifice diameter 0.18mm, hole count 48,18 ± 1 DEG C of temperature of ring blowing, humidity 95 ± 2%, wind speed 0.40-0.45m/s, winding speed
Degree 4290m/min.
Embodiment 2
The first step：By mass, in 100 parts of butyl oxides, the nano-zirconium carbide that 25 parts of particle diameters are 100~300nm is added,
Using horizontal mill, grinding distribution 1h, is obtained nano-zirconium carbide dispersion liquid at room temperature；
Second step：First step gained dispersion liquid is moved into reactor, (consumption is nano silicon carbide to add trimethoxy chlorosilane
The 3wt% of zirconium), 40 DEG C are warming up under agitation, react 1h；
3rd step：Second step gained reaction solution, spray-dried machine are dried.Drying process be feed rate 3.0~
4.0kg/h, 180~190 DEG C of import air temperature, 90~100 DEG C of air temperature of outlet, 0.35~0.40m of air draft speed3/ min, mist
Change 100~120kPa of pressure；
4th step：By mass, 18 parts of organic modification nano-zirconium carbide obtained by the 3rd step is gathered in oneself with 100 parts
Amide resin is extruded through screw extruder melt blending, granulation, and functional agglomerate is obtained.Blending technology is screw speed 150rpm,
Each area's temperature is followed successively by 210 ± 3 DEG C, 250 ± 3 DEG C, 245 ± 3 DEG C, 235 ± 3 DEG C, 180 ± 3 DEG C.
5th step：By mass, 20 parts of functional agglomerate obtained by the 4th step is blended with 80 parts of polycaprolactams, warp
Melting, spinning, stretching, winding are obtained extinction heating nylon fibre, and its performance indications is referring to table 1.Spinning technique is screw speed
45r/min, each area's temperature of screw extruder is followed successively by 262 ± 3 DEG C, 266 ± 3 DEG C, 267 ± 3 DEG C, 270 ± 3 DEG C, 270 ± 3 DEG C,
Orifice diameter 0.18mm, hole count 48,18 ± 1 DEG C of temperature of ring blowing, humidity 95 ± 2%, wind speed 0.40-0.45m/s, winding speed
Degree 4290m/min.
The extinction of table 1 heating polyamide fibre main performance index
| Embodiment 1 | Embodiment 2 | |
| Specification | 44.4dtex/48F | 44.4dtex/48F |
| Organise nano silicon carbide zirconium content (wt%) | 1.07 | 3.05% |
| Intensity (cN/dtex) | 39.8 | 39.0 |
| Elongation at break (%) | 43.8 | 42.1 |
| Line density CV values (%) | 1.08 | 1.12 |
| Boiling water shrinkage (%) | 8.2 | 9.2 |
Embodiment 1, the gained fiber of embodiment 2 are made fabric, fabric specification：Longitude and latitude linear density 44.4dtex, through close
740/10cm, filling density 560/10cm, weight per square meter 61g.Fabric is cut into the sample of 50cm × 50cm, is penetrated in 500W
(irradiation distance 50cm) is irradiated under lamp, the surface temperature in sample centre is determined with infrared temperature sensor (0.1 DEG C of precision),
Every five seconds for example records a temperature, calculates liter temperature value of the sample in 20min, and contrast with same specification common fabric.The suction of each sample
Light heating property test result is shown in accompanying drawing 3, as seen from the figure, under identical irradiation time, with embodiment 1, the institute of embodiment 2
The fabric that fiber is made into is obtained, its surface temperature is higher than same specification common fabric, after being irradiated through 20min, with embodiment 1, implemented
The fabric that the gained fiber of example 2 is made into, 6.3 DEG C higher than same specification common fabric, 7.1 DEG C of its surface temperature.
Claims (9)
1. a kind of nano-zirconium carbide of organic modification, it is characterised in that comprise the following steps：
I. nano-zirconium carbide is added in butyl oxide, at room temperature grinding distribution 1h, nano-zirconium carbide dispersion liquid is obtained；
II. trimethoxy chlorosilane is added in dispersion liquid obtained by step I, stirring is warming up to 40 DEG C, reacts 1h；
III. by reaction solution obtained by step II, spray-dried machine is dried, and is obtained organising for Surface coating trimethoxy silicon and is changed
Property nano-zirconium carbide.
2. the nano-zirconium carbide of organic modification according to claim 1, it is characterized in that：The nano-zirconium carbide it is average
Particle diameter is 100~300nm.
3. the nano-zirconium carbide of organic modification according to claim 1, it is characterized in that：By mass, the butyl oxide
Consumption be 100 parts, nano-zirconium carbide consumption be 20~25 parts, trimethoxy chlorosilane consumption for nano-zirconium carbide 3~
5wt%.
4. the nano-zirconium carbide of organic modification according to claim 1 is used to produce polyamide fibre material, described polyamide fibre material
Material has extinction heating property.
5. a kind of polyamide fibre material, it is characterised in that the nano-zirconium carbide containing the organic modification described in claim 1.
6. a kind of polyamide fibre material of the nano-zirconium carbide of the organic modification comprising described in claim 1, it is characterised in that by such as
Lower section method is produced：
I. organic modification nano-zirconium carbide is blended with into fibre with polycaprolactam, is squeezed through screw extruder melt blending
Go out, granulate, functional agglomerate is obtained；
II. step I gained functional agglomerates are cut into slices with polycaprolactam and is blended, extinction is obtained through melting, spinning, stretching, winding
Heating nylon fibre.
7. method according to claim 6, it is characterized in that：The content of modified Nano zirconium carbide is in described functional agglomerate
10~15wt%.
8. method according to claim 6, it is characterized in that：Described master batch and polycaprolactam section in mass ratio 20/
80~10/90 blendings.
9. method according to claim 6, it is characterized in that：The described nano-zirconium carbide that organises in the nylon fibre
Content be 1.0~3.1wt%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107736644A (en) * | 2017-09-29 | 2018-02-27 | 浙江弘尚智能科技股份有限公司 | One kind heating cotton-padded trousers socks |
| CN108691081A (en) * | 2018-05-17 | 2018-10-23 | 无锡恒诺纺织科技有限公司 | Extinction heat preservation is knitted fabric |
| CN109402765A (en) * | 2018-09-12 | 2019-03-01 | 恒天中纤纺化无锡有限公司 | A kind of heat accumulation thermal nylon staple 6 fibre and preparation method thereof |
| CN109594336A (en) * | 2018-12-06 | 2019-04-09 | 泉州联兴发针织织造有限公司 | A kind of preparation method of extinction heat generating and retention functional fabric |
| CN111005207A (en) * | 2019-11-28 | 2020-04-14 | 江苏品创纺织科技有限公司 | Preparation method of intelligent heat-storage temperature-regulating fabric |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107736644A (en) * | 2017-09-29 | 2018-02-27 | 浙江弘尚智能科技股份有限公司 | One kind heating cotton-padded trousers socks |
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| CN109402765A (en) * | 2018-09-12 | 2019-03-01 | 恒天中纤纺化无锡有限公司 | A kind of heat accumulation thermal nylon staple 6 fibre and preparation method thereof |
| CN109402765B (en) * | 2018-09-12 | 2021-05-07 | 恒天中纤纺化无锡有限公司 | Heat-storage warm-keeping chinlon 6 staple fiber and preparation method thereof |
| CN109594336A (en) * | 2018-12-06 | 2019-04-09 | 泉州联兴发针织织造有限公司 | A kind of preparation method of extinction heat generating and retention functional fabric |
| CN111005207A (en) * | 2019-11-28 | 2020-04-14 | 江苏品创纺织科技有限公司 | Preparation method of intelligent heat-storage temperature-regulating fabric |
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Application publication date: 20170613 |