CN114318570A - Preparation method and application of liquid master batch for cool viscose - Google Patents

Preparation method and application of liquid master batch for cool viscose Download PDF

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CN114318570A
CN114318570A CN202111561875.5A CN202111561875A CN114318570A CN 114318570 A CN114318570 A CN 114318570A CN 202111561875 A CN202111561875 A CN 202111561875A CN 114318570 A CN114318570 A CN 114318570A
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CN114318570B (en
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谢伟
李珊珊
刘向向
干仁聪
王美佳
李腾飞
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Poly Plastic Masterbatch Suzhou Co ltd
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Abstract

The invention greatly reduces the particle diameter of the cool particles which are coarser originally through the grinding process, and the finely ground nano particles are stably dispersed in the liquid by using the coating agent, so that the fine powder is not easy to agglomerate and settle after being finely ground. Under the condition that the powder is added into the fiber in a certain amount, the finer the powder is, the better the powder is dispersed, the better the spinnability is, and the cool feeling performance of the fiber is improved. The spinnability and the physical properties of the fiber can be improved to different degrees by adjusting the pH value to be alkalescent and mechanically defoaming. The liquid master batch for cool viscose fiber prepared by the invention can be added into viscose spinning solution to directly spin cool viscose fiber, and has the advantages of good spinnability, water washing resistance, less pollution, good fiber cool sensitivity, lasting cool performance and the like.

Description

Preparation method and application of liquid master batch for cool viscose
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 fibers mainly focus on chemical fibers produced by a melt spinning method, such as terylene, chinlon, polypropylene and the like. The fibers have the problems of skin incompatibility, air impermeability and the like, and are difficult to apply to some close-fitting textiles.
Viscose fiber is a cellulose fiber obtained by extracting and remolding fiber molecules from natural wood cellulose using "wood" as a raw material. The moisture absorption of the viscose fiber meets the physiological requirements of human skin, and has the characteristics of smoothness, coolness, air permeability, static resistance, ultraviolet resistance, gorgeous color, good dyeing fastness and the like. It has the nature of cotton, the quality of silk, is genuine plant fiber, is derived from nature and is superior to nature. The fabric is widely applied to the fields of various underwear, textile, clothes, non-woven fabrics and the like.
Most of the existing preparation methods of cool viscose fibers are to mix a graphene material and jade powder with a fiber base material respectively and extrude the mixture by a screw to obtain functional master batches containing the graphene material and the jade powder respectively. And then blending the fiber base material and the two functional master batches and then carrying out melt spinning to obtain the cool fiber. The method has the advantages that after the cool master batch is prepared in advance, cool fibers such as terylene/chinlon can be directly prepared through melt spinning, the cool fibers do not need to be finished after printing and dyeing, and the cool fibers are washing-resistant. The disadvantages are that the jade powder is used as a cool medium, the heat conduction effect is poor, and the particle size of the jade powder is thick, so the spinning specification is limited greatly and only heavy denier yarns can be spun.
The improved method is to modify polyamide with modified bamboo powder and nano ZnO as filler to prepare fiber core material, and to use modified nano ALN and nano TiO2The polyurethane is modified to prepare a fiber skin material, and the eccentric skin-core composite fiber is prepared by adopting melt spinning, so that the prepared fiber has the sun-proof and cool functions. The method adopts nano ALN as a cool medium, has better heat conduction effect than jade powder, but the ALN also has the problems of generally larger particle size and the like, and is difficult to disperse in a fiber base material.
The invention aims to prepare the cool liquid master batch through research, the master batch can be directly added into spinning stock solution for spinning, and cool viscose can be directly spun. The underwear fabric prepared from the cool viscose fiber has good washing fastness and good skin-friendly and cool performances.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above problems occurring in the prior art.
Therefore, an object of the present invention is to provide a method for preparing a liquid masterbatch for cool viscose fibers.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions: a method for preparing a liquid master batch for cool viscose fiber 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 the cool powder, and continuously mixing; adding the mixed materials into a sand mill, selecting zirconium beads, performing coarse grinding and then fine grinding to reduce the particle size of the powder to 0.3-0.8 mu m; obtaining a finished cool liquid master batch after vacuum defoaming;
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 defoaming agent, 0-1 part of preservative, 0-1 part of pH regulator, 20-30 parts of cool powder and 60-75 parts of deionized water.
As a preferable embodiment of the method for preparing the liquid masterbatch for cool viscose fiber according to the present invention, wherein: the coating agent comprises but is not limited to one or a combination of more of trimethylolethane, trimethylolpropane, neopentyl glycol, triethanolamine and trimethylamine.
As a preferable embodiment of the method for preparing the liquid masterbatch for cool viscose fiber according to the present invention, wherein: the dispersing agent comprises but is not limited to one or a combination of more of sodium lignosulfonate, sodium lauryl sulfate, calcium alkyl sulfonate, a dispersing agent MF, lauryl polyoxyethylene ether and octadecylamine polyoxyethylene ether.
As a preferable embodiment of the method for preparing the liquid masterbatch for cool viscose fiber according to the present invention, wherein: the antifreeze agent comprises but is not limited to one or the combination of two of ethylene glycol and propylene glycol; the defoaming agent comprises but is not limited to polyether modified organic silicon, polysiloxane and polyoxyethylene, and the combination of the polyether modified organic silicon, the polysiloxane and the polyoxyethylene is one or more.
As a preferable embodiment of the method for preparing the liquid masterbatch for cool viscose fiber according to the present invention, wherein: the preservative comprises but is not limited to one or a combination of more than one of 2-n-octyl-4-isothiazolin-3-one, 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one; the pH adjusting agent includes, but is not limited to, sodium hydroxide, sodium bicarbonate, disodium hydrogen phosphate, organic amines.
As a preferable embodiment of the method for preparing the liquid masterbatch for cool viscose fiber according to the present invention, wherein: the cool powder comprises but is not limited to jade powder, mica powder, crystal powder, boron nitride and alumina, or the combination of more than one of the jade powder, the mica powder, the crystal powder, the boron nitride and the alumina.
As a preferable embodiment of the method for preparing the liquid masterbatch for cool viscose fiber according to the present invention, wherein: the pH regulator includes, but is not limited to, sodium hydroxide, sodium bicarbonate, disodium hydrogen phosphate, and organic amine (AMP95), and the pH of the mixed material is 8-10.
As a preferable embodiment of the method for preparing the liquid masterbatch for cool viscose fiber according to the present invention, wherein: also comprises the following steps of (1) preparing,
the premixing is carried out for 5-10min at 40-50 ℃ and 1500 rpm; the mixing is continued to be stirred for 30-60min at the speed of 2000-2800 rpm;
the coarse grinding is carried out firstly and then the fine grinding is carried out, and the steps of coarse grinding for 10-60min by selecting zirconium beads with the diameter of 0.6-1.0mm and fine grinding for 10-180min by selecting zirconium beads with the diameter of 0.4-0.6mm are also included.
As a preferable embodiment of the method for preparing the liquid masterbatch for cool viscose fiber according to the present invention, wherein: and the vacuum defoaming condition is negative pressure, stirring and defoaming are carried out, the micro bubbles of the liquid color master are removed, and the defoaming time is 2-4 h.
As a preferable example of the use of the liquid masterbatch for cool-feeling viscose fibers according to the present inventionA protocol, wherein: the application can be directly added into spinning stock solution for spinning and spinning cool viscose; the contact cool feeling coefficient of the fabric prepared from the cool viscose fiber is more than or equal to 0.38J/cm2·s。
The invention has the beneficial effects that:
the invention greatly reduces the particle diameter of the cool particles which are coarser originally through the grinding process, and the finely ground nano particles are stably dispersed in the liquid by using the coating agent, so that the fine powder is not easy to agglomerate and settle after being finely ground. Under the condition that the powder is added into the fiber in a certain amount, the finer the powder is, the better the powder is dispersed, the better the spinnability is, and the cool feeling performance of the fiber is improved. The spinnability and the physical properties of the fiber can be improved to different degrees by adjusting the pH value to be alkalescent and mechanically defoaming.
The liquid master batch for cool viscose fiber prepared by the invention can be added into viscose spinning solution to directly spin cool viscose fiber, and has the advantages of good spinnability, water washing resistance, less pollution, good fiber cool sensitivity, lasting cool performance and the like.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
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 than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is 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 for spinning the viscose staple fiber by using the liquid color master comprises the following steps: firstly, adding liquid color master batch into viscose spinning stock solution (the stock solution is strong alkaline, the concentration of sodium hydroxide is 5 wt%) according to a certain proportion, uniformly mixing, quantitatively conveying the mixture to a spinning nozzle through a metering pump through a pipeline, and immersing the spinning nozzle in a 90 ℃ coagulation bath (the coagulation bath is strong in acidity, and the concentration of sulfuric acid is 120 g/L). And (3) solidifying and forming the fiber from the spinning nozzle in an acid coagulating bath, bundling and drafting, and finally preparing the viscose staple fiber through the working procedures of cutting, refining, oiling, drying, packaging and the like.
The polymerization degree of the polyether modified organic silicon used in the embodiment of the invention is as follows: 10-1000 parts; polymerization degree of polysiloxane: 10-2000; polymerization degree of polyoxyethylene: 10-100 parts of; the other raw materials are all sold in the ordinary market unless otherwise specified.
Example 1:
2 parts of sodium lignosulfonate, 0.1% AMP95, 4 parts of ethylene glycol, 0.3 part of polysiloxane, 0.1 part of 1, 2-benzisothiazolin-3-one were added in this order to water and premixed for 5min at 1000rpm at 40 ℃. Then 30 parts of cool powder mixture (mica powder: boron nitride 1: 1) is added, and stirring is continued for 30min at 1500 rpm. And adding the premixed material into a sand mill, selecting zirconium beads with the size of 0.8-1.0mm, coarsely grinding for 30min, and finely grinding the zirconium beads with the size of 0.4-0.6mm for 15 min. The particle size of the cool feeling powder mixture in the cool feeling master batch was measured by using a malvern laser particle sizer, and the average particle size was 0.88 μm. And (4) carrying out vacuum defoaming for 2h under negative pressure to obtain the finished product liquid color master batch.
The liquid color master batch spun-bonded adhesive short fiber is used, so that the mass fraction of the cool feeling powder in the fiber is 1%. The fineness of the short fiber is 1.5dtex, and the dry and wet strength is 1.90cN/dtex and 1.05cN/dtex respectively. After the fibers are 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/cm2·s。
Example 2:
1 part of sodium lignosulphonate, 1 part of lauryl polyoxyethylene ether, 0.3 part of trimethylolethane, 0.1% AMP95, 4 parts of ethylene glycol, 0.3 part of polysiloxane and 0.1 part of 1, 2-benzisothiazolin-3-one are sequentially added into water, and premixed for 5min at 40 ℃ and 1000 rpm. Then 30 parts of cool powder mixture (mica powder: boron nitride 1: 1) is added, and stirring is continued for 30min at 1500 rpm. And adding the premixed material into a sand mill, selecting zirconium beads with the size of 0.8-1.0mm, coarsely grinding for 30min, and finely grinding the zirconium beads with the size of 0.4-0.6mm for 15 min. The particle size of the cool feeling powder mixture in the cool feeling master batch was measured by using a malvern laser particle sizer, and the average particle size was 0.69 μm. And (4) carrying out vacuum defoaming for 2h under negative pressure to obtain the finished product liquid color master batch.
The liquid color master batch spun-bonded adhesive short fiber is used, so that the mass fraction of the cool feeling powder in the fiber is 1%. The fineness of the short fiber is 1.5dtex, and the dry and wet strength is 1.95cN/dtex and 1.08cN/dtex respectively. After the fibers are 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/cm2·s。
Example 3:
adding 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 organic silicon and 0.1 part of 5-chloro-2-methyl-4-isothiazoline-3-ketone into water in sequence, and premixing at 40 ℃ and 1000rpm for 10 min. Then 30 parts of boron nitride powder is added, and stirring is continued at 1500rpm for 30 min. And adding the premixed material into a sand mill, selecting zirconium beads with the size of 0.6-0.8mm, coarsely grinding for 30min, and finely grinding the zirconium beads with the size of 0.3-0.4mm for 15 min. The particle size of the cool feeling powder mixture in the cool feeling master batch was measured by using a malvern laser particle sizer, and the average particle size was 0.41 μm. And (4) carrying out vacuum defoaming for 2h under negative pressure to obtain the finished product liquid color master batch.
The liquid color master batch spun-bonded adhesive short fiber is used, so that the mass fraction of the cool feeling powder in the fiber is 1%. The fineness of the short fiber is 1.5dtex, and the dry and wet strength is 1.98cN/dtex and 1.08cN/dtex respectively. After the fibers are 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/cm2·s。
Example 4:
taking example 3 as an example, the raw material ratios of the cool feeling powder mixtures were changed, the other steps and parameters were the same as those of example 3, and the contact cool feeling of the prepared short fibers was as shown in table 1.
TABLE 1
Figure BDA0003415473230000051
As can be seen from example 4 and table 1, the ratio of mica powder to boron nitride powder in the liquid masterbatch has little influence on the contact cooling coefficient of the fiber material. In fact, as the boron nitride powder has higher heat-conducting property, the more the boron nitride powder is added, 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 size of the cool feeling powder in the liquid color master batch was changed, the other steps and parameters were the same as those of example 3, and the contact cool feeling of the prepared short fiber is shown in table 2.
TABLE 2
Figure BDA0003415473230000061
Under the condition that the powder is added into the fiber in a certain amount, the finer the powder is, the better the spinnability is, and the cool feeling performance of the fiber is improved. The thickness of the cotton viscose fiber is about 1.2-1.5 denier generally, the particle size of the cool feeling powder sold in the market at present is about 5-20 μm generally, and the particle size range is difficult to be applied to spinning 1.2-1.5 denier fiber. Therefore, the cool feeling powder needs to be pre-ground to reduce the particle size to be in the range of 0.4-0.8 μm.
Under the condition that the cool feeling powder content in the fiber is certain, smaller zirconium beads are used, the particle size of the cool feeling powder can be further reduced by prolonging the grinding time, but the cool feeling performance of the fiber cannot be infinitely increased and finally tends to a value. The average particle size is generally selected to be 0.4. mu.m.
Example 6:
taking example 3 as an example, the content of the coating agent in the liquid color masterbatch is changed, other steps and parameters are the same as those in example 3, and the contact cool feeling of the prepared short fiber is shown in table 3.
TABLE 3
Figure BDA0003415473230000071
The particle size of the cool feeling particles which are coarser originally is greatly reduced through a grinding process, and the finely ground nano particles are stably dispersed in the liquid by using the coating agent, so that the fine powder is not easy to agglomerate and settle after being finely ground. The coating agent is matched with the cool powder with small grain size, particularly the coating agent comprises the following components in parts by weight: the cool powder comprises 0.6 parts: at 25, the contact cool feeling coefficient can be improved by 40 percent, the dispersion stability of the cool feeling powder can be kept, and the average grain diameter of the cool 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 is changed, respectively, to spin-bond the adhesive staple fiber. Other steps and parameters were the same as in example 3, and the contact cooling condition of the produced short fibers is shown in Table 4.
TABLE 4
Figure BDA0003415473230000072
Figure BDA0003415473230000081
The liquid color master needs to be adjusted to be alkalescent by a pH regulator, because if the liquid color master is acidic, the addition of the liquid color master into the spinning solution can lead to partial reduction of the alkali cellulose in advance, cause the heterogeneity of the quality of the spinning solution and greatly reduce the spinnability.
Example 8:
the short fibers prepared in examples 1 to 3 were washed with water, respectively, and the washing performance was tested.
TABLE 5
Figure BDA0003415473230000082
The invention greatly reduces the particle diameter of the cool particles which are coarser originally through the grinding process, and the finely ground nano particles are stably dispersed in the liquid by using the coating agent, so that the fine powder is not easy to agglomerate and settle after being finely ground. Under the condition that the powder is added into the fiber in a certain amount, the finer the powder is, the better the powder is dispersed, the better the spinnability is, and the cool feeling performance of the fiber is improved. The spinnability and the physical properties of the fiber can be improved to different degrees by adjusting the pH value to be alkalescent and mechanically defoaming.
The liquid master batch for cool viscose fiber prepared by the invention can be added into viscose spinning solution to directly spin cool viscose fiber, and has the advantages of good spinnability, water washing resistance, less pollution, good fiber cool sensitivity, lasting cool performance and the like.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, 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 modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (10)

1. A preparation method of a liquid master batch for cool viscose fiber is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
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 the cool powder, and continuously mixing; adding the mixed materials into a sand mill, selecting zirconium beads, performing coarse grinding and then fine grinding to reduce the particle size of the powder to 0.3-0.8 mu m; obtaining a finished cool liquid master batch after vacuum defoaming;
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 defoaming agent, 0-1 part of preservative, 0-1 part of pH regulator, 20-30 parts of cool powder and 60-75 parts of deionized water.
2. The method for preparing a liquid masterbatch for cool viscose fiber according to claim 1, wherein: the coating agent comprises but is not limited to one or a combination of more of trimethylolethane, trimethylolpropane, neopentyl glycol, triethanolamine and trimethylamine.
3. The method for preparing a liquid masterbatch for cool viscose fiber according to claim 1, wherein: the dispersing agent comprises but is not limited to one or a combination of more of sodium lignosulfonate, sodium lauryl sulfate, calcium alkyl sulfonate, a dispersing agent MF, lauryl polyoxyethylene ether and octadecylamine polyoxyethylene ether.
4. The method for preparing a liquid masterbatch for cool viscose fiber according to claim 1, wherein: the antifreeze agent comprises but is not limited to one or the combination of two of ethylene glycol and propylene glycol; the defoaming agent comprises but is not limited to polyether modified organic silicon, polysiloxane and polyoxyethylene, and the combination of the polyether modified organic silicon, the polysiloxane and the polyoxyethylene is one or more.
5. The method for preparing a liquid masterbatch for cool viscose fiber according to claim 1, wherein: the preservative comprises but is not limited to one or a combination of 2-n-octyl-4-isothiazolin-3-one, 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one.
6. The method for preparing a liquid masterbatch for cool viscose fiber according to claim 1, wherein: the cool powder comprises but is not limited to jade powder, mica powder, crystal powder, boron nitride and alumina, or the combination of more than one of the jade powder, the mica powder, the crystal powder, the boron nitride and the alumina.
7. The method for preparing a liquid masterbatch for cool viscose fiber according to claim 1, wherein: the pH regulator includes but is not limited to sodium hydroxide, sodium bicarbonate, disodium hydrogen phosphate and organic amine, and the pH of the mixed material is 8-10.
8. The method for preparing a liquid masterbatch for cool viscose fiber according to claim 1, wherein: also comprises the following steps of (1) preparing,
the premixing is carried out for 5-10min at 40-50 ℃ and 1500 rpm; the mixing is continued to be stirred for 30-60min at the speed of 2000-2800 rpm;
the coarse grinding is carried out firstly and then the fine grinding is carried out, and the steps of coarse grinding for 10-60min by selecting zirconium beads with the diameter of 0.6-1.0mm and fine grinding for 10-180min by selecting zirconium beads with the diameter of 0.4-0.6mm are also included.
9. The method for preparing a liquid masterbatch for cool viscose fiber according to claim 1, wherein: and the vacuum defoaming condition is negative pressure, stirring and defoaming are carried out, the micro bubbles of the liquid color master are removed, and the defoaming time is 2-4 h.
10. The application of the liquid master batch for the cool viscose fiber is characterized in that: the application can be directly added into spinning stock solution for spinning and spinning cool viscose; the contact cool feeling coefficient of the fabric prepared from the cool viscose fiber is more than or equal to 0.38J/cm2·s。
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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
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