CN114318570B - Preparation method and application of liquid master batch for cool viscose fiber - Google Patents
Preparation method and application of liquid master batch for cool viscose fiber Download PDFInfo
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- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 claims description 3
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- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 2
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Abstract
The invention greatly reduces the original coarser cool powder particle size through the grinding process, and the coating agent is used for stably dispersing the ground nano particles in the liquid, so that the powder is not easy to agglomerate and settle after grinding. Under the condition that the amount of the powder added into the fiber is fixed, the finer the powder is, the better the dispersion is, the better the spinnability is, and the cool feeling of the fiber is improved. The pH is adjusted to be weak alkaline, and mechanical defoaming can improve the spinnability of the fiber and the physical properties of the fiber to different degrees. The liquid master batch for cool viscose fiber prepared by the invention can be added into viscose spinning stock solution to directly spin cool viscose fiber, and has the advantages of good spinnability, water washing resistance, less pollution, good cool feeling of fiber, long cool feeling and the like.
Description
Technical Field
The invention belongs to the technical field of functional liquid master batches, and particularly relates to a preparation method of a liquid master batch for cool viscose fibers.
Background
Most researches on cool feeling fibers are mainly focused on chemical fibers produced by a melt spinning method, such as terylene, chinlon, polypropylene fibers and the like. These fibers themselves present some problems of skin-friendliness, air-impermeability, etc., and are often difficult to apply in some personal textiles.
Viscose fiber, which is cellulose fiber obtained by taking 'wood' as a raw material, extracting and remolding fiber molecules from natural wood cellulose. The moisture absorption of the viscose fiber meets the physiological requirement of human skin, and has the characteristics of smoothness, coolness, ventilation, static resistance, ultraviolet resistance, gorgeous color, better color fastness and the like. It has cotton nature, silk quality, is a genuine plant fiber, and is derived from nature and superior to natural. At present, the method is widely applied to the fields of various underwear, textile, clothing, non-woven and the like.
The existing preparation method of cool sense viscose fiber is to mix graphene material and jade powder with fiber base material respectively, and extrude the mixture by screw to obtain functional master batch containing the graphene material and functional master batch containing the jade powder respectively. And then blending the fiber base material with the two functional master batches, and then melt spinning to obtain the cool fiber. The method has the advantages that the cool feeling master batch can be prepared in advance, and then the cool feeling fibers such as terylene/chinlon can be directly prepared through melt spinning, so that the after-finishing of printing and dyeing is not needed, and the method is wash-resistant. The defect is that the jade powder is used as cool medium, the heat conduction effect is poor, and the particle size of the jade powder is thick, so that the specification of spinning is limited greatly, and only coarse denier yarns can be spun.
The improved method is to prepare fiber core material by modifying polyamide with modified bamboo powder and nano ZnO as filler, and simultaneously using modified nano ALN and nano TiO 2 The polyurethane is modified to prepare the fiber skin material, and the eccentric skin-core composite fiber is prepared by melt spinning, so that the prepared fiber has sun-proof and cool feeling functions. The method adopts nanometer ALN as cool medium, has better heat conduction effect than jade powder, but ALN also has the problems of general larger particle size and the like, and is difficult to disperse in fiber base materials.
The invention aims to prepare a cool liquid master batch through research, and the master batch can be directly added into spinning stock solution for spinning, so that cool viscose fiber can be directly spun. The underwear fabric prepared from cool feeling viscose fiber has good washing resistance, skin friendliness and cool feeling.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used to limit the scope of the invention.
The present invention has been made in view of the above-mentioned and conventional problems occurring in the prior art.
Accordingly, the invention aims to provide a preparation method of a liquid master batch for cool viscose fiber.
In order to solve the technical problems, according to one aspect of the present invention, the following technical solutions are provided: a preparation method of a liquid master batch for cool sense viscose fiber, which comprises the following steps,
adding a coating agent, a dispersing agent, an antifreeze agent, a defoaming agent, a preservative and a pH regulator into deionized water for premixing, adding cool feeling powder, and continuing mixing; adding the mixed materials into a sand mill, and selecting zirconium beads for coarse grinding and fine grinding to reduce the particle size of the powder to 0.3-0.8 mu m; vacuum defoamation to obtain a finished cool liquid master batch;
the liquid master batch comprises 0-1 part of coating agent, 0-5 parts of dispersing agent, 0-5 parts of antifreeze agent, 0-1 part of defoamer, 0-1 part of preservative, 0-1 part of pH regulator, 20-30 parts of cool feeling powder and 60-75 parts of deionized water.
As a preferable scheme of the preparation method of the liquid master batch for cool viscose fiber, the invention comprises the following steps: the coating agent comprises one or a combination of several of trimethylolethane, trimethylolpropane, neopentyl glycol, triethanolamine and trimethylamine.
As a preferable scheme of the preparation method of the liquid master batch for cool viscose fiber, the invention comprises the following steps: the dispersing agent comprises one or a combination of several of sodium lignin sulfonate, sodium lauryl sulfate, calcium alkyl sulfonate, dispersing agent MF, dodecyl polyoxyethylene ether and octadecyl amine polyoxyethylene ether.
As a preferable scheme of the preparation method of the liquid master batch for cool viscose fiber, the invention comprises the following steps: the antifreeze agent comprises one or two of ethylene glycol and propylene glycol; the defoamer comprises one or a combination of several of polyether modified organosilicon, polysiloxane and polyoxyethylene.
As a preferable scheme of the preparation method of the liquid master batch for cool viscose fiber, the invention comprises the following steps: the preservative comprises one or a combination of several of 2-n-octyl-4-isothiazolin-3-ketone, 2-methyl-4-isothiazolin-3-ketone and 5-chlorine-2-methyl-4-isothiazolin-3-ketone; the pH regulator includes, but is not limited to, sodium hydroxide, sodium bicarbonate, disodium hydrogen phosphate, organic amines.
As a preferable scheme of the preparation method of the liquid master batch for cool viscose fiber, the invention comprises the following steps: the cool sense powder comprises one or a combination of more than one of jade powder, mica powder, crystal powder, boron nitride and aluminum oxide.
As a preferable scheme of the preparation method of the liquid master batch for cool viscose fiber, the invention comprises the following steps: the pH regulator includes, but is not limited to, sodium hydroxide, sodium bicarbonate, disodium hydrogen phosphate, organic amine (AMP 95), and the pH of the mixed materials is 8-10.
As a preferable scheme of the preparation method of the liquid master batch for cool viscose fiber, the invention comprises the following steps: also included is a method of manufacturing a semiconductor device,
the premixing is performed at 40-50deg.C and 1000-1500rpm for 5-10min; the mixing is carried out at 2000-2800rpm for 30-60min;
the steps of rough grinding and then fine grinding comprise that zirconium beads with the diameter of 0.6-1.0mm are selected for rough grinding for 10-60min, and zirconium beads with the diameter of 0.4-0.6mm are selected for fine grinding for 10-180min.
As a preferable scheme of the preparation method of the liquid master batch for cool viscose fiber, the invention comprises the following steps: the vacuum defoaming condition is negative pressure, defoaming is carried out while stirring, microbubbles of the liquid color master are removed, and the defoaming time is 2-4h.
As a preferable scheme of the application of the liquid master batch for cool viscose fiber, the invention comprises the following steps: the application can be directly added into the spinning solution for spinning and spinning cool viscose fiber; fabric prepared from cool viscose fiber with contact cool feeling coefficient more than or equal to 0.38J/cm 2 ·s。
The invention has the beneficial effects that:
the invention greatly reduces the original coarser cool powder particle size through the grinding process, and the coating agent is used for stably dispersing the ground nano particles in the liquid, so that the powder is not easy to agglomerate and settle after grinding. Under the condition that the amount of the powder added into the fiber is fixed, the finer the powder is, the better the dispersion is, the better the spinnability is, and the cool feeling of the fiber is improved. The pH is adjusted to be weak alkaline, and mechanical defoaming can improve the spinnability of the fiber and the physical properties of the fiber to different degrees.
The liquid master batch for cool viscose fiber prepared by the invention can be added into viscose spinning stock solution to directly spin cool viscose fiber, and has the advantages of good spinnability, water washing resistance, less pollution, good cool feeling of fiber, long cool feeling and the like.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The preparation method of the viscose staple fiber spun by using the liquid color masterbatch comprises the following steps: firstly, adding the liquid color master batch into viscose spinning stock solution (the stock solution is strong alkaline and the concentration of sodium hydroxide is 5 wt%) according to a certain proportion, uniformly mixing, quantitatively conveying the mixture to a spinneret through a pipeline by a metering pump, and immersing the spinneret in a coagulating bath (the coagulating bath is strong acid and the concentration of sulfuric acid is 120 g/L) at 90 ℃. The fiber coming out of the spinneret is solidified and formed in an acidic coagulating bath, is subjected to bundling and drafting, and is finally prepared into viscose staple fiber through the procedures of cutting, refining, oiling, drying, packaging and the like.
Polymerization degree of polyether modified organosilicon used in the embodiment of the invention: 10-1000; degree of polymerization of polysiloxane: 10-2000; polymerization degree of polyoxyethylene: 10-100; the other raw materials are all commonly and commercially available unless otherwise specified.
Example 1:
to water was added 2 parts of sodium lignin sulfonate, 0.1% AMP95, 4 parts of ethylene glycol, 0.3 parts of polysiloxane, 0.1 parts of 1, 2-benzisothiazolin-3-one in this order, and the mixture was premixed at 1000rpm for 5 minutes at 40 ℃. Then, 30 parts of cool powder mixture (mica powder: boron nitride=1:1) was added thereto, and stirring was continued for 30 minutes at 1500 rpm. Adding the premixed material into a sand mill, coarsely grinding zirconium beads with the size of 0.8-1.0mm for 30min, and finely grinding zirconium beads with the size of 0.4-0.6mm for 15min. The particle size of the cool powder mixture in the cool master batch was measured using a malvern laser particle sizer, and the average particle size was 0.88 μm. And vacuum defoamating for 2 hours under negative pressure to obtain the finished product liquid color master batch.
The liquid color masterbatch is used for spinning the viscose staple fiber, so that the mass fraction of cool powder in the fiber is 1%. The fineness of the obtained staple fibers was 1.5dtex, and the dry and wet strengths were 1.90cN/dtex and 1.05cN/dtex, respectively. After the fiber is woven into the fabric, the cool feeling performance is tested according to GB/T35263, and the contact cool feeling coefficient Qmax is more than or equal to 0.22J/cm 2 ·s。
Example 2:
1 part of sodium lignin sulfonate, 1 part of dodecanol polyoxyethylene ether, 0.3 part of trimethylolethane, 0.1 percent of AMP95, 4 parts of ethylene glycol, 0.3 part of polysiloxane and 0.1 part of 1, 2-benzisothiazolin-3-one are added into water in sequence, and premixed for 5 minutes at 40 ℃ and 1000 rpm. Then, 30 parts of cool powder mixture (mica powder: boron nitride=1:1) was added thereto, and stirring was continued for 30 minutes at 1500 rpm. Adding the premixed material into a sand mill, coarsely grinding zirconium beads with the size of 0.8-1.0mm for 30min, and finely grinding zirconium beads with the size of 0.4-0.6mm for 15min. The particle size of the cool powder mixture in the cool master batch was measured using a malvern laser particle sizer, and the average particle size was 0.69 μm. And vacuum defoamating for 2 hours under negative pressure to obtain the finished product liquid color master batch.
The liquid color masterbatch is used for spinning the viscose staple fiber, so that the mass fraction of cool powder in the fiber is 1%. The fineness of the obtained staple fibers was 1.5dtex, and the dry and wet strengths were 1.95cN/dtex and 1.08cN/dtex, respectively. After the fiber is woven into the fabric, the cool feeling performance is tested according to GB/T35263, and the contact cool feeling coefficient Qmax is more than or equal to 0.26J/cm 2 ·s。
Example 3:
3 parts of octadecylamine polyoxyethylene ether, 0.4 part of trimethylamine, 0.1 part of AMP95, 3 parts of ethylene glycol, 0.3 part of polyether modified organosilicon and 0.1 part of 5-chloro-2-methyl-4-isothiazolin-3-one are sequentially added into water and premixed for 10 minutes at 40 ℃ and 1000 rpm. Then 30 parts of boron nitride powder is added, and stirring is continued for 30min at 1500 rpm. Adding the premixed material into a sand mill, coarsely grinding zirconium beads with the size of 0.6-0.8mm for 30min, and finely grinding zirconium beads with the size of 0.3-0.4mm for 15min. The particle size of the cool powder mixture in the cool master batch was measured using a malvern laser particle sizer, and the average particle size was 0.41 μm. And vacuum defoamating for 2 hours under negative pressure to obtain the finished product liquid color master batch.
The liquid color masterbatch is used for spinning the viscose staple fiber, so that the mass fraction of cool powder in the fiber is 1%. The fineness of the obtained staple fibers was 1.5dtex, and the dry and wet strengths were 1.98cN/dtex and 1.08cN/dtex, respectively. After the fiber is woven into the fabric, the cool feeling performance is tested according to GB/T35263, and the contact cool feeling coefficient Qmax is more than or equal to 0.38J/cm 2 ·s。
Example 4:
taking example 3 as an example, the raw material ratios of the cool feeling powder mixture were respectively changed, and the contact cool feeling conditions of the prepared short fibers are shown in table 1, with the other steps and parameters being the same as those of example 3.
TABLE 1
From example 4 and table 1, it is clear that the ratio of mica powder to boron nitride powder in the liquid master batch has little effect on the contact cooling coefficient of the fiber material. In fact, as the boron nitride powder has higher heat conduction performance, the more the adding amount of the boron nitride powder is, the better the contact cool feeling coefficient of the short fiber can be improved.
Example 5:
taking example 3 as an example, the initial average particle diameter of the cool feeling powder in the liquid color master batch was changed, and the contact cool feeling of the prepared staple fibers was as shown in table 2, except that the procedure and parameters were the same as those of example 3.
TABLE 2
Under the condition that the amount of the powder added into the fiber is fixed, the finer the powder is, the better the spinnability is, and the cool feeling of the fiber is improved. The cotton viscose fiber has a general thickness of about 1.2-1.5 denier, the currently marketed cool sense powder particle size is generally thicker, generally about 5-20 μm, and the particle size range is difficult to be applied to spinning 1.2-1.5 denier fiber. Therefore, the cool powder needs to be pre-ground to reduce the particle size to be in the range of 0.4-0.8 mu m.
Under the condition that the content of the cool feeling powder in the fiber is certain, the particle size of the cool feeling powder can be further reduced by using smaller zirconium beads and prolonging the grinding time, but the cool feeling performance of the fiber cannot be infinitely increased and finally tends to be a value. The average particle size is generally selected to be 0.4. Mu.m.
Example 6:
using example 3 as an example, the film coating agent content in the liquid color master batch was changed, and the contact cooling feeling of the prepared staple fibers was as shown in Table 3 in the same manner as in example 3.
TABLE 3 Table 3
The original coarser cool powder particle size is greatly reduced by the grinding process, and the ground nano particles are stably dispersed in the liquid by using the coating agent, so that the powder is not easy to agglomerate and settle after grinding. The coating agent is matched with cool powder with small particle size, and particularly comprises the following components in parts by weight: the cool feeling powder is 0.6: at 25, the contact cooling feeling coefficient can be improved by 40%, and the dispersion stability of the cooling feeling powder can be maintained, so that the average particle size of the cooling feeling powder in the liquid color master batch is still maintained at the level of 0.5 mu m after the liquid color master batch is placed for 1 month.
Example 7:
taking example 3 as an example, the pH of the liquid color master was changed, and viscose staple fibers were spun. Other steps and parameters were the same as in example 3, and the contact cooling feeling of the prepared staple fibers was as shown in Table 4.
TABLE 4 Table 4
The liquid color master needs to be made weak alkaline by a pH regulator, because if the liquid color master is acidic, the addition of the liquid color master to the spinning solution can lead to the early partial reduction of alkali cellulose, so that the quality of the spinning solution is uneven, and the spinnability is also greatly reduced.
Example 8:
the short fibers prepared in examples 1 to 3 were washed with water, respectively, and the washing performance was measured.
TABLE 5
The invention greatly reduces the original coarser cool powder particle size through the grinding process, and the coating agent is used for stably dispersing the ground nano particles in the liquid, so that the powder is not easy to agglomerate and settle after grinding. Under the condition that the amount of the powder added into the fiber is fixed, the finer the powder is, the better the dispersion is, the better the spinnability is, and the cool feeling of the fiber is improved. The pH is adjusted to be weak alkaline, and mechanical defoaming can improve the spinnability of the fiber and the physical properties of the fiber to different degrees.
The liquid master batch for cool viscose fiber prepared by the invention can be added into viscose spinning stock solution to directly spin cool viscose fiber, and has the advantages of good spinnability, water washing resistance, less pollution, good cool feeling of fiber, long cool feeling and the like.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (6)
1. A preparation method of a liquid master batch for cool viscose fiber is characterized by comprising the following steps: the method comprises the following steps:
adding coating agent, dispersing agent, antifreeze agent, defoamer, preservative and pH regulator into deionized water
Premixing the ingredients, adding cool powder, and continuously mixing; adding the mixed materials into a sand mill, and selecting zirconium beads for coarse grinding and fine grinding to reduce the particle size of the powder to 0.3-0.8 mu m; vacuum defoamation to obtain a finished cool liquid master batch;
the liquid master batch comprises 0.4-1 part of coating agent, 3-5 parts of dispersing agent, 3-5 parts of antifreeze agent, 0.3-1 part of defoamer, 0.1-1 part of preservative, 0.1-1 part of pH regulator, 20-30 parts of cool feeling powder and 60-75 parts of deionized water;
the coating agent comprises one or more of trimethylolethane, trimethylolpropane, neopentyl glycol, triethanolamine and trimethylamine;
the pH regulator comprises sodium hydroxide, sodium bicarbonate, disodium hydrogen phosphate and organic amine, and the pH value of the mixed materials is 8-10;
the premixing is performed at 40-50deg.C and 1000-1500rpm for 5-10min; the mixing is carried out at 2000-2800rpm for 30-60min;
the steps of rough grinding and then fine grinding comprise that zirconium beads with the diameter of 0.6-1.0mm are selected for rough grinding for 10-60min, and zirconium beads with the diameter of 0.4-0.6mm are selected for fine grinding for 10-180min;
the vacuum defoaming condition is negative pressure, defoaming is carried out while stirring, microbubbles of the liquid color master are removed, and the defoaming time is 2-4h.
2. The method for preparing the liquid master batch for cool viscose fiber according to claim 1, which is characterized in that: the dispersing agent comprises one or a combination of more of sodium lignin sulfonate, sodium lauryl sulfate, calcium alkyl sulfonate, a dispersing agent MF, dodecyl polyoxyethylene ether and octadecyl amine polyoxyethylene ether.
3. The method for preparing the liquid master batch for cool viscose fiber according to claim 1, which is characterized in that: the antifreeze agent comprises one or two of ethylene glycol and propylene glycol; the defoamer comprises one or a combination of more of polyether modified organic silicon, polysiloxane and polyoxyethylene.
4. The method for preparing the liquid master batch for cool viscose fiber according to claim 1, which is characterized in that: the preservative comprises one or a combination of more than one of 2-n-octyl-4-isothiazolin-3-ketone, 2-methyl-4-isothiazolin-3-ketone and 5-chlorine-2-methyl-4-isothiazolin-3-ketone.
5. The method for preparing the liquid master batch for cool viscose fiber according to claim 1, which is characterized in that: the cool sense powder comprises one or a combination of more of jade powder, mica powder, crystal powder, boron nitride and aluminum oxide.
6. The application of the liquid master batch for cool viscose fiber prepared by the preparation method of the liquid master batch for cool viscose fiber according to any one of claims 1-5, which is characterized in that: the application can be directly added into the spinning solution for spinning and spinning cool viscose fiber; fabric prepared from cool viscose fiber with contact cool feeling coefficient not less than 0.38J/cm 2 ·s。
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| CN101805934A (en) * | 2010-04-02 | 2010-08-18 | 山东海龙股份有限公司 | Ice-cold viscose fiber and preparation method thereof |
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| CN110644067A (en) * | 2019-10-16 | 2020-01-03 | 苏州世名科技股份有限公司 | Flame-retardant slurry for viscose stock solution spinning and preparation method thereof |
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| CN101805934A (en) * | 2010-04-02 | 2010-08-18 | 山东海龙股份有限公司 | Ice-cold viscose fiber and preparation method thereof |
| CN106222776A (en) * | 2016-07-27 | 2016-12-14 | 恒天海龙（潍坊）新材料有限责任公司 | A kind of jade is felt nice and cool regenerated celulose fibre and preparation method thereof |
| CN110644067A (en) * | 2019-10-16 | 2020-01-03 | 苏州世名科技股份有限公司 | Flame-retardant slurry for viscose stock solution spinning and preparation method thereof |
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