CN102776600B - Method for preparing efficient far infrared nylon fibers - Google Patents
Method for preparing efficient far infrared nylon fibers Download PDFInfo
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- CN102776600B CN102776600B CN2012102379102A CN201210237910A CN102776600B CN 102776600 B CN102776600 B CN 102776600B CN 2012102379102 A CN2012102379102 A CN 2012102379102A CN 201210237910 A CN201210237910 A CN 201210237910A CN 102776600 B CN102776600 B CN 102776600B
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- far infrared
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Abstract
The invention relates to a method for preparing efficient far infrared nylon fibers, comprising the steps of (1) preparing soluble magnesium salt and soluble aluminum salt into a mixed aqueous solution; adding the mixed aqueous solution drop by drop to a NaOH/Na2CO3 solution; and after crystallizing, leaching, washing and drying to obtain Mg-Al-CO3 LDHs; (2) calcinating the Mg-Al-CO3 LDHs at a high temperature to obtain MMO; (3) drying polyamide 6 chips, mixing the polyamide 6 chips with the MMO evenly, blending and granulating to obtain far infrared master-batch chips; and (4) drying the far infrared master-batch chips with forced draught in vacuum, and finally performing melt spinning to obtain the far infrared nylon fibers. The method for preparing the efficient far infrared nylon fibers is simple in preparation process and low in cost; and the prepared far infrared functional nylon fibers are of good mechanical property and excellent far infrared emission rate, can promote human blood circulation and improve immunity, and has good heat-preservation and health care effects.
Description
Technical field
The invention belongs to the preparation field of functional nylon fibre, particularly a kind of preparation method of efficient far infrared nylon fibre.
Background technology
Society, people more and more pay attention to healthy, and functional textile also has been given more concerns.The production scale of differentialand functional fiber is also increasing, mainly comprise fire-retardant, antibiotic, antistatic, uvioresistant, far IR fibre etc., have warming, the health care specific function far IR fibre as a kind of fibre in differentiation, the title that " fiber of life " arranged, the far IR fibre goods also are described as the health products that the 21 century mankind need most, and have wide practical value and application prospect.Japanese, Russian, German etc. start the research and development of this technology, especially Japanology in the eighties in 20th century the earliest, product is also abundanter.The domestic-developed far-infrared fabric starts from the beginning of the nineties, and the performance of product has been compared a certain distance with Japan and other countries.
Under normal temperature, the ceramic powder of far infrared transmissivity more than 65% can be used as the far-infrared functional material, a lot of inorganic matters, as oxide, carbide, boride etc. all have the far infrared radiation characteristic, yet the infrared emittance of one matter is low, generally select the mixture of many oxide to make the far-infrared functional material.Layered double-hydroxide (layed double hydroxides) LDHs is a kind of anionic clay of layer structure, has special layer structure and physicochemical properties.(Rives, Materials Chemistry and Physics, 2002,75:19) structure of LDHs is very similar to shepardite Mg (OH)
2, by MgO
6the octahedra prismatic that shares becomes elementary layer, Mg
2+be positioned at octahedral center, OH
-be positioned at octahedral summit, these octahedrons planar are piled into two-dimentional layer.(Goh, Lim, Dong, Water Research, 2008,42:1343-1368) LDHs changes MMO into after high-temperature calcination.We have mentioned magnesia and aluminium oxide itself is exactly far-infrared ceramic powder commonly used before this, similarly, MMO also can be used as the new far infrared nano-powder, and, in composite oxides, both even mixing can be widened their far infrared transmissivities in broadband more, have also given its new potential application.Wang etc. have reported Mg-Al-CO
3lDHs and Mg-Al-DIA LDHs add to respectively in the LDPE plastic sheeting for farm use, and its result shows, adds the almost not change of LDPE plastic sheeting for farm use light transmission rate of these two kinds of LDHs, but to 1428-400cm
-1the INFRARED ABSORPTION effect remarkable.LDHs and MMO thereof are at 400-1500cm
-1wave band has strong INFRARED ABSORPTION, have excellent INFRARED ABSORPTION performance (Wang, et al., Journal of Solid State Chemistry, 2010,183,1114-1119).Therefore, MMO is added in polymeric matrix and can give the performance that polymer is new, important application prospect is arranged on the high-performance far IR fibre.Especially, the far infrared nylon fibre also lacks large-scale production and application, and exploitation far infrared polyamide fibre Related product has huge potential value.
Polyamide fibre is one of principal item of synthetic fiber, is again polyamide fiber, is commonly called as nylon.Polyamide fibre is with containing amide groups (CONH on main chain
-) be connected to alkyl the synthetic fiber that the linear polyamide of construction unit is made.Regularly arranged due to nylon on molecular structure, large intermolecular energy forms many hydrogen bond structures, makes it have high-crystallinity, at aspects such as mechanical property, chemical property, hot propertys, has advantages of outstanding.The principal item of polyamide fibre is nylon 66 and nylon 6.Nylon 6 is output maximums in the nylon kind at present, and the nylon 6 of usining prepares the far infrared nylon fibre as raw material, has wide market prospects and using value.
In the preparation of far IR fibre, mainly have at present following problem: after the large and heterogeneity of the particle diameter of far infrared additive, powder processing process loaded down with trivial details, fiber spinnability is poor and the fiber surface harsh hand is poor.Therefore, the efficient far infrared functional fibre of development of new becomes development trend.At present the particle diameter that forms after the LDHs high-temperature calcination is little and MMO that be evenly distributed adds in fiber also report of preparation far infrared nylon fibre to.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of efficient far infrared nylon fibre, the method technique is simple, with low cost, be easy to suitability for industrialized production, the far infrared nylon fibre mechanical property of preparation is good, far infrared transmissivity is high, can be for developing the far infrared, warm, health care goods of function admirable.
The preparation method of a kind of efficient far infrared nylon fibre of the present invention comprises:
(1) Mg-Al-CO
3the preparation of LDHs:
Solubility magnesium salts and aluminum soluble salt are mixed with to mixed aqueous solution, then dropwise join NaOH/Na
2cO
3(NaOH and Na
2cO
3mass ratio be 4:5) in solution, then, at 80 ~ 100 ℃ of crystallization 2 ~ 6h, suction filtration, washing, oven dry obtain Mg-Al-CO
3lDHs;
(2) preparation of MMO:
By above-mentioned Mg-Al-CO
3lDHs, through 400 ~ 600 ℃ of high-temperature calcination 3 ~ 5h, loses hydroxyl and CO
3 2-obtain the MMO(alloy and belong to oxide, mixed metal oxide);
(3) preparation of far-infrared matrix:
By after polyamide 6 section vacuumize, with above-mentioned MMO, evenly mix, the blend granulation obtains the far-infrared matrix section;
(4) preparation of far infrared nylon fibre
By above-mentioned far-infrared matrix section, through the vacuum forced air drying, finally on the twin-screw composite spinning machine, melt spinning obtains the far infrared nylon fibre.
Solubility magnesium salts described in step (1) is MgCl
26H
2o, aluminum soluble salt is AlCl
36H
2o.
NaOH/Na described in step (1)
2cO
3the pH value of solution is 12 ~ 14.
The Mg-Al-CO that step (1) obtains
3in LDHs, the mol ratio of Mg element and Al element is 2:1.
1 ~ 4wt% that described in step (3), the addition of MMO is polyamide 6 section.
Described in step (3), vacuum drying temperature is 100 ~ 130 ℃, and the time is 12 ~ 36h.
Described in step (4), the temperature of vacuum forced air drying is 100 ~ 140 ℃.
Spinning temperature described in step (4) is 265 ~ 290 ℃, and speed is 3500～8000m/min.
The far infrared normal emittance of the far infrared nylon fibre obtained in step (4) is 87.3%.
The present invention adds composite metal oxide (mixed metal oxide, MMO) in polyamide 6, through blend granulation, melt spinning, obtains a kind of new and effective far infrared nylon fibre; The selected far infrared additive of the present invention is the MMO obtained through 400 ~ 600 ℃ of calcinings by layered double-hydroxide (LDHs).
Mg-Al composite oxide of the present invention, its component mainly comprises MgO and Al
2o
3the simple mixtures that is different from both, this composite oxides are to be prepared from by the calcining of LDHs presoma, there is high dispersion and uniformity between two kinds of compositions, overcome the problem that traditional far-infrared ceramic powder exists, improved the far infrared transmissivity of fibre, when addition is 2wt%, prepared nylon fibre is 87.3% through on IR-1 type far infrared transmissivity measuring instrument, recording its normal emittance of far infrared at the 8-14 mu m waveband.
The magnalium MMO that the present invention adopts magnalium LDHs to obtain high-specific surface area through high-temperature calcination, as the far infrared additive, makes the far infrared nylon fibre with the polyamide 6 blend melt spinning.The MMO particle diameter that prepared magnalium LDHs specific area is high, obtain after calcining is little, distribution uniform.
Beneficial effect:
(1) preparation technology of the present invention is simple, with low cost, has huge using value and wide market prospects, is easy to realize suitability for industrialized production;
(2) the present invention is usingd magnalium LDHs and is decomposed the magnalium MMO obtain as the far infrared additive, obtained a kind of new and effective far-infrared functional nylon fibre through blend, spinning, there is good mechanical property and excellent far infrared transmissivity, its far infrared normal emittance is 87.3%, can promote blood circulation of human body, improve immunity, there is good warming, health-care effect.
The accompanying drawing explanation
Fig. 1 .Mg-Al-CO
3the X-ray diffractogram of LDHs and MMO;
The N of Fig. 2 .MMO
2adsorption-desorption isothermal curve and pore-size distribution;
Fig. 3. preparation technology's flow chart of efficient far infrared nylon fibre of the present invention;
Fig. 4. the stereoscan photograph on efficient far infrared nylon fibre of the present invention surface.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only are not used in and limit the scope of the invention for the present invention is described.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Take 51g MgCl under room temperature
26H
2o and 45g AlCl
36H
2o, join 265 ml H by both
2be made into mixed solution in O, dropwise join NaOH/Na
2cO
3in solution (pH=14), in 90 ℃ of lower crystallization 4h suction filtration, washing, oven dry, obtain Mg-Al-CO
3lDHs.Mg-Al-CO by preparation
3lDHs calcines 4h and obtains MMO under 500 ℃, takes 10kg polyamide 6 section 120 ℃ of dry 12h in vacuum drying oven.MMO is joined to dried polyamide 6 section and mixes by the 2wt% of polymer chips, and in double screw extruder, the blend granulation obtains the far-infrared functional master batch.Finally cut into slices through 120 ℃ of vacuum forced air dryings, and melt spinning obtains the far infrared nylon fibre on the twin-screw composite spinning machine, spinning temperature is 275 ℃, and spinning speed is 3500m/min.
Fig. 1 is Mg-Al-CO prepared by the present embodiment
3the X-ray diffractogram of LDHs and Mg-Al composite oxide MMO.As can be seen from the figure, after calcining, layer structure is destroyed, and loses interlayer moisture, carbonate and interlayer hydroxyl, obtains magnesia and aluminium oxide and disperses powder highly uniformly.
Embodiment 2
Take 51g MgCl under room temperature
26H
2o and 45g AlCl
36H
2o, join 265ml H by both
2be made into mixed solution in O, dropwise join NaOH/Na
2cO
3in solution (pH=12) at 80 ℃ of lower crystallization 6h, and suction filtration, washing, oven dry obtain Mg-Al-CO
3lDHs.Mg-Al-CO prepared by coprecipitation
3lDHs obtains MMO at 500 ℃ of lower high-temperature calcination 4h, takes 8kg polyamide 6 section 120 ℃ of dry 24h in vacuum drying oven.MMO is joined to dried polyamide 6 section and mixes by the 3wt% of polymer chips, and in double screw extruder, the blend granulation obtains the far-infrared functional master batch.Finally cut into slices through 120 ℃ of vacuum forced air dryings, and melt spinning obtains the far infrared nylon fibre on the twin-screw composite spinning machine, spinning temperature is 265 ℃, and spinning speed is 4000m/min.
Fig. 2 is Mg-Al-CO prepared by the present embodiment
3the N of the MMO that LDHs obtains through high-temperature calcination
2adsorption-desorption isothermal curve and corresponding pore size distribution curve, its specific area is 180m
2/ g.
Embodiment 3
Take 51g MgCl under room temperature
26H
2o and 45g AlCl
36H
2o, join 265ml H by both
2be made into mixed solution in O, dropwise join NaOH/Na
2cO
3in solution (pH=14), in 80 ℃ of lower crystallization 6h suction filtration, washing, oven dry, obtain Mg-Al-CO
3lDHs.Mg-Al-CO by preparation
3lDHs obtains MMO at 400 ℃ of lower high-temperature calcination 5h, takes 10kg polyamide 6 section 110 ℃ of dry 36h in vacuum drying oven.MMO is joined to dried polyamide 6 section and mixes by the 3wt% of polymer chips, and in double screw extruder, the blend granulation obtains the far-infrared functional master batch.Finally cut into slices through 120 ℃ of vacuum forced air dryings, and melt spinning obtains the far infrared nylon fibre, spinning temperature is 280 ℃, and spinning speed is 3500m/min.
Preparation technology's flow chart that Fig. 3 is new and effective far infrared nylon fibre in the present embodiment, adopt full comminution granulation to prepare the far infrared nylon fibre.Fig. 4 is the SEM figure of this experimental example mid and far infrared nylon fibre without silk noil, can find out that this additive has good dispersiveness at fiber surface.
Embodiment 4
Take 51g MgCl under room temperature
26H
2o and 45g AlCl
36H
2o, join 265ml H by both
2be made into mixed solution in O, dropwise join NaOH/Na
2cO
3in solution (pH=10), in 100 ℃ of lower crystallization 2h suction filtration, washing, oven dry, obtain Mg-Al-CO
3lDHs.Mg-Al-CO by preparation
3lDHs obtains MMO at 400 ℃ of lower high-temperature calcination 3h, takes 10kg polyamide 6 section 110 ℃ of dry 24h in vacuum drying oven.MMO is joined to dried polyamide 6 section and mixes by the 3wt% of polymer chips, and in double screw extruder, the blend granulation obtains the far-infrared functional master batch.Finally cut into slices through 120 ℃ of vacuum forced air dryings, and melt spinning obtains the far infrared nylon fibre, spinning temperature is 275 ℃, and spinning speed is 5000m/min.
Embodiment 5
Take 51g MgCl under room temperature
26H
2o and 45g AlCl
36H
2o, join 265ml H by both
2be made into mixed solution in O, dropwise join NaOH/Na
2cO
3in solution (pH=10), in 90 ℃ of lower crystallization 3h suction filtration, washing, oven dry, obtain Mg-Al-CO
3lDHs.Mg-Al-CO by preparation
3lDHs obtains MMO at 600 ℃ of lower high-temperature calcination 4h, takes 10kg polyamide 6 section 130 ℃ of dry 12h in vacuum drying oven.MMO is joined to dried polyamide 6 section and mixes by the 3wt% of polymer chips, and in double screw extruder, the blend granulation obtains the far-infrared functional master batch.Finally cut into slices through 120 ℃ of vacuum forced air dryings, and melt spinning obtains the far infrared nylon fibre, spinning temperature is 265 ℃, and spinning speed is 8000m/min.
Claims (7)
1. the preparation method of an efficient far infrared nylon fibre comprises:
(1) solubility magnesium salts and aluminum soluble salt are mixed with to mixed aqueous solution, then dropwise join NaOH/Na
2cO
3in solution, then, at 80～100 ℃ of crystallization 2～6h, suction filtration, washing, oven dry obtain Mg-Al-CO
3lDHs; Mg-Al-CO
3in LDHs, the mol ratio of Mg element and Al element is 2:1;
(2) by above-mentioned Mg-Al-CO
3lDHs, through 400～600 ℃ of high-temperature calcination 3～5h, obtains MMO;
(3) by after polyamide 6 section vacuumize, with above-mentioned MMO, evenly mix, the blend granulation obtains the far-infrared matrix section;
(4) by the forced air drying of above-mentioned far-infrared matrix section process vacuum, last melt spinning obtains the far infrared nylon fibre, and the far infrared normal emittance of the far infrared nylon fibre wherein obtained is 87.3%.
2. the preparation method of a kind of efficient far infrared nylon fibre according to claim 1, it is characterized in that: the solubility magnesium salts described in step (1) is MgCl
26H
2o, aluminum soluble salt is AlCl
36H
2o.
3. the preparation method of a kind of efficient far infrared nylon fibre according to claim 1, is characterized in that: the NaOH/Na described in step (1)
2cO
3the pH value of solution is 12～14.
4. the preparation method of a kind of efficient far infrared nylon fibre according to claim 1, it is characterized in that: described in step (3), vacuum drying temperature is 100～130 ℃, the time is 12～36h.
5. the preparation method of a kind of efficient far infrared nylon fibre according to claim 1, is characterized in that: 1～4wt% that described in step (3), the addition of MMO is polyamide 6 section.
6. the preparation method of a kind of efficient far infrared nylon fibre according to claim 1, it is characterized in that: described in step (4), the temperature of vacuum forced air drying is 100～140 ℃.
7. the preparation method of a kind of efficient far infrared nylon fibre according to claim 1, it is characterized in that: the temperature of the melt spinning described in step (4) is 265～290 ℃, speed is 3500～8000m/min.
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| CN104233501B (en) * | 2014-08-29 | 2016-04-27 | 广东新会美达锦纶股份有限公司 | A kind of preparation method of the far infrared PA6 fiber containing multiple inorganic particle |
| CN105297180A (en) * | 2015-11-13 | 2016-02-03 | 昆山华阳新材料股份有限公司 | Manufacturing process of PET/PTT composite fiber |
| CN105297171A (en) * | 2015-11-13 | 2016-02-03 | 昆山华阳新材料股份有限公司 | Manufacturing process of biologic elastic polyester fiber |
| CN105755566A (en) * | 2016-03-02 | 2016-07-13 | 张家港市安顺科技发展有限公司 | Method for producing far-infrared chinlon short fiber |
| CN106245199A (en) * | 2016-10-31 | 2016-12-21 | 李宏龙 | Microcirculqtory system far infrared fabric (AB cloth) |
| US20210130982A1 (en) | 2018-07-04 | 2021-05-06 | The Hong Kong Research Institute Of Textiles And Apparel Limited | Application of profiled fiber in infrared radiation material and textiile |
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| CN102433763B (en) * | 2011-08-26 | 2013-10-16 | 中国纺织科学研究院 | Functional fiber, manufacturing method and fabric formed via weaving functional fiber |
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