CN109930226A - A kind of high thermal conductivity viscose rayon composite material and preparation method - Google Patents
A kind of high thermal conductivity viscose rayon composite material and preparation method Download PDFInfo
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Abstract
The invention belongs to the preparation field of functional fiber, in particular to a kind of high thermal conductivity viscose rayon composite material and preparation method.The present invention provides a kind of high thermal conductivity viscose rayon composite material, and the component of the composite material includes viscose rayon and hydroxylating boron nitride, wherein the quality of hydroxylating boron nitride is 5~60wt% of composite material quality.The highly filled thermally conductive viscose glue dimension composite material of gained of the invention in the axial direction of fiber there is considerable thermal coefficient, fiber itself also to maintain good hydrophilicity, so as to assign the good heat-conductive characteristic of fabric and moisture pick-up properties, possibility is provided for practical application of this thermally conductive viscose rayon in terms of fabric.
Description
Technical field:
The invention belongs to the preparation field of functional fiber, in particular to a kind of high thermal conductivity viscose rayon composite material and its
Preparation method.
Background technique:
Human body heat management, especially body temperature lowering technology are concerned in recent years, it can allow people in hot environment
Silk silk slight chill in the air can be still experienced, so that people be allowed to feel body and mind pleasure.Body temperature lowering technology relies primarily on air-conditioning at present
Refrigeration, it needs to consume a large amount of energy while refrigeration and the temperature in entire room all lowers, and is unfavorable for sustainable development
Exhibition.Compared to air conditioner refrigerating, the fabric by dressing functionalization lowers the temperature of body part, is a kind of very economical, section
The mode of energy, receives the extensive concern of researcher.
The heat dissipation of fabric at present relies primarily on three kinds of heat radiation, heat transfer and heat exchange modes.For current textile material
Such as polyester fiber, terylene, acrylic fibers, especially viscose rayon, they due to near infrared light do not have good permeability,
The thermal coefficient of itself is also very low, so the heat dissipation of this kind fabric relies primarily on moisture absorption, ventilative mode, heat dissipation effect is bad,
Discomfort is brought to wearer under hot environment.Do not change fiber it is hygroscopic under the premise of, assign fiber it is better
Heating conduction is conducive to the surface that the heat that human body generates is transmitted to fabric by fabric by way of heat transfer, then pass through
The mode of heat exchange and heat radiation radiates with external environment, to realize effective control to human body temperature.
International and national is still in infancy about the research of conductive fabric at present, and is needed not in most of method
The organic solvent of environmental protection, and preparation method can not also be popularized on a large scale.In view of the foregoing drawbacks, it develops biodegradable thermally conductive
The large-scale preparation method of viscose rayon has great importance for the practical application of conductive fabric.
Summary of the invention:
In view of the foregoing drawbacks, the present invention provides a kind of high thermal conductivity viscose rayon composite material and preparation methods.This hair
Bright method is environmentally protective, preparation process is simple, it is low for equipment requirements, be applicable to industrialized expanding production；Gained height is filled out
Fill thermally conductive viscose glue dimension composite material fiber axial direction have considerable thermal coefficient, fiber itself also maintain it is good
Hydrophilicity is this thermally conductive viscose rayon in fabric so as to assign the good heat-conductive characteristic of fabric and moisture pick-up properties
The practical application of aspect provides possibility.
Technical solution of the present invention:
The invention solves first technical problem be to provide a kind of high thermal conductivity viscose rayon composite material, it is described compound
The component of material includes viscose rayon and hydroxylating boron nitride, wherein the quality of hydroxylating boron nitride is composite material quality
5~60wt%.
Further, the high thermal conductivity viscose rayon composite material is made using following methods: by the cellulose of viscose rayon
Solution is uniformly mixed with hydroxylating boron nitride by churned mechanically mode, and the spinning solution of stably dispersing is obtained, then by wet
High thermal conductivity viscose rayon composite material is prepared in the mode of method spinning.
Further, in the above method, churned mechanically stirring rate is 500~1000rpm.
Further, the cellulose solution of the viscose rayon is made using following methods: using urea and alkali (sodium hydroxide
Or lithium hydroxide) Aqueous Low Temperature mixing of viscose fiber cellulosic material, then recycle to obtain by thawing colourless
Transparent cellulose solution.
Further, the hydroxylating boron nitride using following methods be made: in six side's layered nitride boron be added urea and
Deionized water obtains mixture, is then uniformly dispersed at room temperature by ball-milling treatment to mixture and makes six side's layered nitride boron
By hydroxylating, remaining urea and the boron nitride not being completely exfoliated and drying are finally removed, obtains the modified nitridation of hydroxylating
Boron；Wherein, the amount ratio of hexagonal boron nitride, urea and deionized water is 500~20000mg:30~60g:12~24mL.
Further, in the preparation method of above-mentioned hydroxylating boron nitride, 2~12h of ball-milling treatment at room temperature.
Further, described to remove remaining urea and impurity and dry in the preparation method of above-mentioned hydroxylating boron nitride
Method are as follows: the mixture after ball milling is diluted with deionized water, the nitridation B solution after dilution is repeated at room temperature dilute
Release-operation of ultrasonic disperse-centrifugal treating to remove extra urea and impurity, then lower sediment is taken to dry.
Further, in the preparation method of above-mentioned hydroxylating boron nitride, ball-milling treatment process conditions are as follows: every ball milling 25~
5~20min of the interval 35min.
Further, in the preparation method of above-mentioned hydroxylating boron nitride, in ultrasonic disperse processing, ultrasonic power is 80~
120W, ultrasonic time are 30~40min.
The invention solves second technical problem be to provide the preparation side of above-mentioned high thermal conductivity viscose rayon composite material
Method, the preparation method is that: the cellulose solution of viscose rayon is mixed with hydroxylating boron nitride by churned mechanically mode
Uniformly, the spinning solution of stably dispersing is obtained, high thermal conductivity viscose rayon composite wood is then prepared by way of wet spinning
Material.
Further, in the above method, churned mechanically stirring rate is 500~1000rpm.
Further, in the above method, in wet spinning technology: extruded velocity is 0.66mm/min~12m/min, draw ratio
It is 1~2.
Preparation method described further includes the following steps:
1) it prepares hydroxylating boron nitride: urea is added in six side's layered nitride boron and deionized water obtains mixture, then
It is uniformly dispersed at room temperature by ball-milling treatment to mixture and makes six side's layered nitride boron by hydroxylating, finally removed remaining
Urea and the boron nitride not being completely exfoliated and drying, obtain the modified boron nitride of hydroxylating；Wherein, hexagonal boron nitride, urea
Amount ratio with deionized water is 500~20000mg:30~60g:12~24mL；
2) cellulose solution is prepared: with the Aqueous Low Temperature of urea and alkali (sodium hydroxide or lithium hydroxide) dissolution cellulose
Then raw material recycles to obtain colorless and transparent cellulose solution by thawing；
3) above-mentioned cellulose solution is uniformly mixed with hydroxylating boron nitride by churned mechanically mode, it is steady obtains dispersion
Then viscose glue/boron nitride heat conducting fiber of high thermal conductivity is prepared in fixed spinning solution by way of wet spinning；Wherein, hydroxyl
The content of base boron nitride is 5-60wt%.
Beneficial effects of the present invention:
1, the method for modifying operating process that uses of the present invention is simple, no pollution to the environment, the requirement to appointed condition are low, can
Suitable for industrialized expanding production.
2, the viscose glue of high thermal conductivity prepared by the present invention/boron nitride heat conducting fiber have objective axial thermal conductivity coefficient and preferably
Hydrophily, can assign fabric extraordinary heat-conductive characteristic, can be effectively reduced the temperature of human body surface, realize people
The purpose of body cooling.
3, the viscose glue of high thermal conductivity prepared by the present invention/boron nitride heat conducting fiber is environmentally protective, biodegradable, is conducive to replace
For traditional polyester fiber, terylene, acrylic fibers etc., alleviate white pollution.
Detailed description of the invention:
Fig. 1 (a, b) is the TEM figure of the gained modified boron nitride of hydroxylating in embodiment 1, and Fig. 1 (c, d) is embodiment 1
The XPS analysis of the modified obtained boron nitride of gained hydroxylating is as a result, Fig. 1 (e) is 1 gained hydroxyl of original boron nitride and embodiment
The TGA of the modified obtained boron nitride of baseization is as a result, Fig. 1 (f) is that original boron nitride and 1 gained hydroxylating of embodiment are modified
The XRD result of obtained boron nitride.
Fig. 2 (a) be the apparent viscosity of spinning solution as a result, Fig. 2 (b) be in embodiment 1 60wt% boron nitride spinning solution and
Stability result after the placement of boron nitride aqueous solution 7 days, Fig. 2 (c) are 1 gained viscose rayon of embodiment/boron nitride composite
Contact angle result.
Fig. 3 (a, b) is respectively that viscose rayon/boron nitride composite of the different boron nitride contents of gained in embodiment 1 is answered
Stress-strain curve and mechanical property as a result, Fig. 3 (c, d) be respectively in embodiment 1 gained different orientation degree viscose rayon/
Boron nitride composite stress-strain diagram and mechanical property result.
Fig. 4 is viscose rayon/boron nitride of different stretch ratio under viscose rayon and 60wt% in embodiment 1 and comparative example 1
The heating conduction of composite material.
Fig. 5 (a) is viscose glue/boron nitride heat conducting fiber fabric in embodiment 2 and commercialized cotton fabric category in human-body radiating
Outside drawing in comparative experiments；Fig. 5 (b) is viscose glue/nitridation heat conducting fiber fabric and commercialized cotton fabric category in human-body radiating
It is shown in comparative experiments with the effect that infrared thermal imaging is observed.
Specific embodiment:
The present invention provides a kind of preparation method of high thermal conductivity viscose glue/boron nitride fiber, and the method can be used including as follows
The implementation method of step:
(1) hydroxylating of boron nitride is modified: urea is added in six side's layered nitride boron and deionized water obtains mixture, so
Ball-milling treatment is uniformly dispersed to mixture and makes six side's layered nitride boron by hydroxylating at room temperature afterwards, finally removes remaining
Urea and the boron nitride not being completely exfoliated and drying obtain the modified boron nitride of hydroxylating；Wherein, hexagonal boron nitride, urea and
The amount ratio of deionized water is 500~20000mg:30~60g:12~24mL；
(2) dissolution in low temperature of cellulose: using urea, sodium hydroxide (or lithium hydroxide) dissolution in low temperature cellulosic material, leads to
It crosses multiple Frozen-thawed cycled and obtains colorless and transparent cellulose solution；
(3) above-mentioned cellulose solution and hydroxylating boron nitride the preparation of spinning solution and heat conducting fiber: are passed through into intense mechanical
The mode of stirring is uniformly mixed, and obtains the spinning solution of stably dispersing, high thermal conductivity is then prepared by way of wet spinning
Viscose glue/boron nitride heat conducting fiber；Wherein, the content of hydroxylating boron nitride is 5-60wt%.
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.
Embodiment 1
High thermal conductivity viscose glue/boron nitride fiber is prepared using following steps:
Step 1: the hydroxylating of boron nitride is modified:
30g urea and 12mL deionized water are added in 500mgBNNS powder, then uses planetary ball mill at room temperature
Ball milling 10h, specifically, every ball milling 30min interval 10min, amounts to ball milling 10h；By product that ball milling obtains with 1000mL go from
Sub- water is diluted, and by the nitridation B solution after dilution, ultrasound 30min disperses under conditions of room temperature, ultrasonic power are 100W
It is centrifuged after uniformly, revolving speed is 3000rpm, centrifugation time 15min, supernatant after centrifugation when centrifugation；By supernatant
With deionized water filtering and washing 4 times or more, the product after multiple washing is placed in vacuum drying oven and is dried
Obtain hydroxylating boron nitride.
Step 2: the dissolution in low temperature of cellulose:
By 80.4g deionized water, 15g urea, 4.6g lithium hydroxide is maintained at -12 DEG C after mixing, then glues 6g
The cellulosic material cotton linter paper pulp of glue fiber is added in above-mentioned cryogenic fluid, by more under the stirring of 500-1000rpm
Secondary Frozen-thawed cycled obtains colorless and transparent cellulose solution.
Step 3: the preparation of spinning solution and heat conducting fiber:
Hydroxylating boron nitride (EOH-BNNS) in step 1 and the cellulose solution in step 2 are pressed into hydroxylating nitrogen respectively
Changing boron content is that (i.e. hydroxylating boron nitride accounts for composite material by 5wt%, 10wt%, 20wt%, 40wt%, 60wt% and 80wt%
The accounting of gross mass) 500-1000rpm stirring rate be stirred it is uniformly mixed, obtain mobility it is stable white spin
Silk liquid, is then prepared under each hydroxylating boron nitride content by way of wet spinning: respectively in low extruded velocity
(0.66mm/min) and high extruded velocity (12m/min), draw ratio be respectively 1,1.5 and 2 viscose rayon/boron nitride it is compound
Material finally obtains final product with deionized water foam washing 4h and vacuum drying.
Embodiment 2
High thermal conductivity viscose glue/boron nitride fiber is prepared using following steps:
Step 1: the hydroxylating of boron nitride is modified:
30g urea and 12mL deionized water are added in 1500mgBNNS powder, then uses planetary type ball-milling at room temperature
Machine ball milling 16h, specifically, every ball milling 30min interval 10min, amounts to ball milling 16h；The product 1000mL that ball milling is obtained
Deionized water is diluted, by the nitridation B solution after dilution under conditions of room temperature, ultrasonic power are 100W ultrasound 30min
It is centrifuged after being uniformly dispersed, revolving speed is 3000rpm, centrifugation time 15min, supernatant after centrifugation when centrifugation；It will be upper
Product after multiple washing is placed in vacuum drying oven and is dried with deionized water filtering and washing 4 times or more by clear liquid,
Hydroxylating boron nitride can be obtained.
Step 2: the dissolution in low temperature of cellulose:
By 80.4g deionized water, 15g urea, 4.6g sodium hydroxide is maintained at -12 DEG C after mixing, then by 6g fibre
It ties up plain raw material cotton linter paper pulp to be added in above-mentioned cryogenic fluid, be stirred under 500-1000rpm stirring rate and by multiple
Frozen-thawed cycled obtains colorless and transparent cellulose solution.
Step 3: the preparation of spinning solution and heat conducting fiber:
It is by hydroxylating boron nitride content by the hydroxylating boron nitride in step 1 and the cellulose solution in step 2
60wt% is uniformly mixed in 500-1000rpm, obtains the stable white spinning solution of mobility, is then existed by wet process mode
Viscose rayon/boron nitride composite that draw ratio is respectively 1,1.5 and 2 is prepared under high extruded velocity (12m/min), finally
Final product is obtained with deionized water foam washing 4h and vacuum drying.
Comparative example 1
A kind of viscose rayon, is prepared using following steps:
Step 1: the dissolution in low temperature of cellulose:
By 80.4g deionized water, 15g urea, 4.6g sodium hydroxide is maintained at -12 DEG C after mixing, then by 6g fibre
It ties up plain raw material to be added in above-mentioned cryogenic fluid, recycles to obtain colorless and transparent fiber by thawing in 500-1000rpm
Plain solution.
Step 2: the preparation of viscose rayon:
Then cellulose solution in step 1 is prepared by way of wet spinning viscose rayon, finally use deionization
Bubble, which is washed 4h and is dried in vacuo, obtains final product.
Performance test:
The present invention has carried out the test of HRTEM, XPS, TGA and XRD to gained hydroxyl boron nitride in embodiment 1, as a result such as
Shown in Fig. 1.As can be seen from Figure 1 complete hexagonal crystal is able to maintain in hydroxylating boron nitride (EOH-BNNS) face of the present invention
Type structure, and there is the defect of some lattices at edge, illustrates that the functional group of ball milling modification has been grafted on the side of hydroxylating boron nitride
Edge, from XPS analysis it can be found that there is O atom to be grafted on above B atom, it was demonstrated that hydroxylating boron nitride is edge hydroxylating
Reaction, and hydroxy radical content can also react, hydroxylating boron nitride maintains well in 1.5wt% from XRD from TGA
(002) and (004) crystal face peak, so ball milling modification is on thermal coefficient in boron nitride face almost without very big influence.
In addition also obtained spinning fluid viscosity, spinning solution stability and wet spinning in embodiment 1 are obtained viscous
Glue fiber/boron nitride composite has carried out water contact angle characterization, as a result as shown in Figure 2.Find out from Fig. 2 (a), due to hydroxyl
Good interaction between base boron nitride and cellulose, even if hydroxylating boron nitride/cellulose spinning fluid can be made to exist
Good mobility is still maintained under the content of 60wt%, viscosity is not obviously improved；And this hydroxylating boron nitride
The spinning solution that content is 60wt% is placed after 7 days without any sedimentation, it was demonstrated that spinning solution is highly stable (such as
Shown in Fig. 2 b), but hydroxylating boron nitride itself can not then be stablized 7 days in aqueous solution under identical concentration, bottom
There is apparent precipitating.In addition, since hydroxylating boron nitride inherently has good hydrophily, so with its content
Increase, the hydrophily of viscose rayon gradually improves, after the stretch since the surface of viscose rayon is more smooth, so table
Face water contact angle further declines, and viscose glue/boron nitride fiber water contact angle of final 60wt% can be down to 24 °, to guarantee
Fiber good hygroscopicity.In Fig. 2, RCF, L-60%, H-60%, H-60%-1.5, H-60%-2 respectively represent pure glue
Glue fiber (RCF), low extruded velocity-hydroxylating boron nitride content are 60% (L-60%), high extruded velocity-hydroxylating nitrogenizes
Boron content is that 60%- draw ratio is 1 (H-60%), and high extruded velocity-hydroxylating boron nitride content is that 60%- draw ratio is 1.5
(H-60%-1.5), high extruded velocity-hydroxylating boron nitride content is viscose glue/nitrogen that 60%- draw ratio is 2 (H-60%-2)
Change boron composite fibre.
Fig. 3 is that viscose rayon/boron nitride of different hydroxylating boron nitride contents and different stretch ratio is compound in embodiment 1
The mechanical property of material.It can be found that with the increase of hydroxylating boron nitride content, viscose glue/boron nitride fiber mechanical strength
Be gradually reduced with extension at break, but downward trend before 60wt% all than more gentle, the viscose glue of 60wt%/boron nitride is fine
Dimension still can keep preferable mechanical strength and elongation at break.And when viscose glue/boron nitride fiber of 60wt% is by rear end
After stretching orientation, the tensile strength of fiber is further obviously improved, and can achieve 140MPa, has approached the drawing of viscose rayon
Stretch intensity.
Fig. 4 characterizes viscose rayon/nitrogen of different stretch ratio under viscose rayon and 60wt% in embodiment 1 and comparative example 1
Change the heating conduction of boron composite material.It can be found that original viscose rayon thermal coefficient is lower than 1, but due to high thermal conductivity hydroxyl
The addition for changing boron nitride, can be obviously improved its heating conduction, and with the increase of draw ratio, viscose glue/nitrogen of final 60wt%
The axial thermal conductivity coefficient for changing boron fibre can be up to 2.9W/m K.
Viscose rayon/boron nitride composite that Fig. 5 is the 60wt% that draw ratio is 2 under high extruded velocity in embodiment 1
It has been made into one piece of fabric, and has been compared with commercialized cotton fabric category.We by their two surfaces for being attached to skin, to
It after its surface temperature is stablized, is observed with infrared thermal imaging, the viscose glue of 60wt% obtained by the discovery embodiment of the present invention is fine
The fabric surface temperature that dimension/boron nitride composite is made into is 2.5 DEG C higher than cotton fabric category, is more nearly the temperature of skin surface,
Therefore viscose glue/boron nitride fiber of 60wt% can be effectively by the surface of the heat transfer of skin to fabric, by effective
Heat radiation and heat exchange radiate to skin.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. high thermal conductivity viscose rayon composite material, which is characterized in that the component of the composite material includes viscose rayon and hydroxyl
Change boron nitride, wherein the quality of hydroxylating boron nitride is 5~60wt% of composite material quality.
2. high thermal conductivity viscose rayon composite material according to claim 1, which is characterized in that the high thermal conductivity viscose rayon
Composite material is made using following methods: the cellulose solution of viscose rayon and hydroxylating boron nitride are passed through churned mechanically side
Formula is uniformly mixed, and obtains the spinning solution of stably dispersing, high thermal conductivity viscose rayon is then prepared by way of wet spinning
Composite material.
3. high thermal conductivity viscose rayon composite material according to claim 2, which is characterized in that the churned mechanically stirring
Rate is 500~1000rpm.
4. described in any item high thermal conductivity viscose rayon composite materials according to claim 1~3, which is characterized in that the hydroxyl
Change boron nitride to be made using following methods: urea is added in six side's layered nitride boron and deionized water obtains mixture, then exists
It is uniformly dispersed at room temperature by ball-milling treatment to mixture and makes six side's layered nitride boron by hydroxylating, finally remove remaining urine
Element and the boron nitride not being completely exfoliated and drying obtain the modified boron nitride of hydroxylating；Wherein, it hexagonal boron nitride, urea and goes
The amount ratio of ionized water is 500~20000mg:30~60g:12~24mL.
5. high thermal conductivity viscose rayon composite material according to claim 4, which is characterized in that at room temperature ball-milling treatment 2~
12h。
6. described in any item high thermal conductivity viscose rayon composite materials according to claim 1~5, which is characterized in that the viscose glue
The cellulose solution of fiber is made using following methods: with the cellulose of urea and the Aqueous Low Temperature mixing of viscose fiber of alkali original
Material, then recycles to obtain colorless and transparent cellulose solution by thawing.
7. the preparation method of the described in any item high thermal conductivity viscose rayon composite materials of claim 1~6, which is characterized in that institute
It states the preparation method comprises the following steps: the cellulose solution of viscose rayon is uniformly mixed with hydroxylating boron nitride by churned mechanically mode,
The spinning solution of stably dispersing is obtained, high thermal conductivity viscose rayon composite material is then prepared by way of wet spinning.
8. the preparation method of high thermal conductivity viscose rayon composite material according to claim 7, which is characterized in that mechanical stirring
Stirring rate be 500~1000rpm.
9. the preparation method of high thermal conductivity viscose rayon composite material according to claim 7 or 8, which is characterized in that wet process
In spinning technique: extruded velocity is 0.66mm/min~12m/min, and draw ratio is 1~2.
10. according to the preparation method of the described in any item high thermal conductivity viscose rayon composite materials of claim 7~9, feature exists
In the preparation method includes the following steps:
1) it prepares hydroxylating boron nitride: urea is added in six side's layered nitride boron and deionized water obtains mixture, then in room
Temperature is lower to be uniformly dispersed to mixture by ball-milling treatment and makes six side's layered nitride boron by hydroxylating, and remaining urea is finally removed
The boron nitride not being completely exfoliated and drying obtain the modified boron nitride of hydroxylating；Wherein, hexagonal boron nitride, urea and go from
The amount ratio of sub- water is 500~20000mg:30~60g:12~24mL；
2) it prepares cellulose solution: dissolving cellulosic material with the Aqueous Low Temperature of urea and alkali, then followed by thawing
Ring obtains colorless and transparent cellulose solution；
3) above-mentioned cellulose solution is uniformly mixed with hydroxylating boron nitride by churned mechanically mode, obtains stably dispersing
Then viscose glue/boron nitride heat conducting fiber of high thermal conductivity is prepared in spinning solution by way of wet spinning；Wherein, hydroxylating
The content of boron nitride is 5~60wt%.
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| CN112981582A (en) * | 2021-02-09 | 2021-06-18 | 华中科技大学 | Temperature control fiber integrating heat superconducting and refrigerating functions and preparation method and application thereof |
| CN113005766A (en) * | 2021-03-29 | 2021-06-22 | 江南大学 | Processing method of fiber product with cool feeling |
| CN113002082A (en) * | 2021-02-07 | 2021-06-22 | 中国科学院合肥物质科学研究院 | Biomass-based high-thermal-conductivity flexible composite membrane and preparation method thereof |
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