CN108950730A - It is a kind of to prepare silicon carbide nanometer line/alginic acid composite fibre spinning process - Google Patents
It is a kind of to prepare silicon carbide nanometer line/alginic acid composite fibre spinning process Download PDFInfo
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- CN108950730A CN108950730A CN201810812178.4A CN201810812178A CN108950730A CN 108950730 A CN108950730 A CN 108950730A CN 201810812178 A CN201810812178 A CN 201810812178A CN 108950730 A CN108950730 A CN 108950730A
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- China
- Prior art keywords
- silicon carbide
- nanometer line
- carbide nanometer
- alginic acid
- sodium alginate
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 68
- 239000000835 fiber Substances 0.000 title claims abstract description 61
- 229960001126 alginic acid Drugs 0.000 title claims abstract description 36
- 239000000783 alginic acid Substances 0.000 title claims abstract description 36
- 229920000615 alginic acid Polymers 0.000 title claims abstract description 36
- 235000010443 alginic acid Nutrition 0.000 title claims abstract description 26
- 150000004781 alginic acids Chemical class 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000009987 spinning Methods 0.000 title claims abstract description 22
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000661 sodium alginate Substances 0.000 claims abstract description 33
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 33
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 33
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000000908 ammonium hydroxide Substances 0.000 claims description 8
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 5
- 230000001112 coagulating effect Effects 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 230000015271 coagulation Effects 0.000 claims description 2
- 238000005345 coagulation Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002070 nanowire Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 19
- 239000000243 solution Substances 0.000 abstract description 15
- 238000002347 injection Methods 0.000 abstract description 11
- 239000007924 injection Substances 0.000 abstract description 11
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000002166 wet spinning Methods 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract 1
- 239000002657 fibrous material Substances 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 25
- 238000005259 measurement Methods 0.000 description 15
- 239000000523 sample Substances 0.000 description 10
- 238000002513 implantation Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- LCWAOCHOPBSGMU-UHFFFAOYSA-J aluminum;magnesium;sodium;hydrogen carbonate;oxygen(2-);silicon;trihydroxide Chemical compound [OH-].[OH-].[OH-].[O-2].[Na+].[Mg+2].[Al+3].[Si].OC([O-])=O LCWAOCHOPBSGMU-UHFFFAOYSA-J 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 235000012149 noodles Nutrition 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/04—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of alginates
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Fibers (AREA)
Abstract
Silicon carbide nanometer line/alginic acid complex fiber material spinning process is prepared the invention discloses a kind of.The present invention is by wet spinning technology, by sodium alginate soln through abundant predissolve, dissolution, then it is mixed into sodium alginate soln and silicon carbide nanometer line, and by being sufficiently mixed, obtain well dispersed silicon carbide nanometer line/sodium alginate spinning solution, above-mentioned spinning solution is injected into calcium chloride solution through digital injection pump, silicon carbide nanometer line/alginic acid composite fibre is made in naturally dry at room temperature.Preparation method process controllability of the invention is strong, easy to operate, is suitble to large-scale production, and product intensity obtained is high, and for true tensile strength up to 7.9N, lowest resistance value is 2.1 × 10‑11Ω。
Description
Technical field
The present invention relates to a kind of preparation methods of composite fibre, and in particular to a kind of to prepare silicon carbide nanometer line/alginic acid
The spinning process of fiber.
Background technique
Alginic acid fibre is, using wet spinning, sodium alginate soln to be squeezed by spinneret orifice using sodium alginate as raw material
Enter in the coagulating bath containing divalent metal, then a kind of natural polymer being process through processes such as washing, drawing-off, sizings
Sub-functionality fiber, has that high-hygroscopicity, biocompatibility, flexibility is good, tensile property is good etc., and excellent properties, application are very wide
It is general, but the electric property of alginic acid fibre, heating conduction and chemical stability are poor, constrain its answering in textile industry
With.Silicon carbide nanometer line have good chemical stability, wearability, corrosion resistance, heating conduction, electromagnetic wave absorption performance with
And the features such as mechanical performance.
Based on this, the excellent properties of the two are combined together, prepare excellent thermal conductivity and there is electromagnetic shielding performance
Functional fiber be of great significance to the application of wearable device and field of textile industry, and ground there is presently no relevant
Study carefully and reports.
Summary of the invention
In order to solve the problems in background technique, to prepare silicon carbide nanometer line/alginic acid compound the present invention provides a kind of
The spinning process of fiber, using wet spinning technology, process controllability is strong.
The present invention adopts the following technical scheme that
The present invention the following steps are included:
1) pretreatment of silicon carbide nanometer line: silicon carbide nanometer line is rinsed after mixed acid is handled with deionized water, through taking out
Deionized water, ammonium hydroxide and polyethylene glycol 400 is added after filter drying to be placed in baking oven and react, then is configured to carbon after filtering drying
SiClx nanowire solution is spare；
2) it prepares sodium alginate soln: first sodium alginate being added in deionized water, stirring and dissolving, then exists at normal temperature
It is stirred under heating condition up to required sodium alginate soln；
3) it prepares silicon carbide nanometer line/sodium alginate spinning solution: the pretreated silicon carbide nanometer line of step 1) is added
Enter in the sodium alginate soln prepared to step 2) to get required silicon carbide nanometer line/sodium alginate spinning solution；
4) prepare silicon carbide nanometer line/alginic acid as-spun fibre: the spinning solution that step 3) is obtained is carried out through coagulating bath
Up to required silicon carbide nanometer line/alginic acid as-spun fibre after solidification；
5) prepare silicon carbide nanometer line/alginic acid composite fibre: the as-spun fibre that step 4) is obtained passes through naturally dry
Afterwards up to required silicon carbide nanometer line/alginic acid composite fibre.
In the step 1), mixed acid is the sulfuric acid and nitric acid of volume ratio 3:1；Deionized water, ammonium hydroxide and polyethylene glycol 400
Volume ratio be 500:30:3, wherein the volume of polyethylene glycol 400 be 0.3 milliliter, deionized water, ammonium hydroxide and polyethylene glycol 400
After addition, the mass fraction of silicon carbide nanometer line solution is 0.3%.
In the step 2), the stirring at normal temperature time is 2 hours, 80-12 DEG C of heating stirring temperature, and mixing time is that 1-3 is small
When, the mass fraction for the sodium alginate soln being prepared is 3-5%.
In the step (3), the volume ratio of silicon carbide nanometer line solution and sodium alginate soln is 1:0.5-2.
In the step (4), coagulating bath is the calcium chloride water that mass fraction is 5%.
In the step (4), spinning solution temperature is 25 DEG C, and coagulation bath temperature is 20-35 DEG C.
In the step (5), the naturally dry time is 3-8 hours.
Beneficial effects of the present invention:
Agents useful for same of the present invention is commercial paraphernalia, is not necessarily to cumbersome preparation, and the required equal mature preparation process of raw material is simple easy
?；Preparation process of the present invention is controllable, easy to operate, and product intensity obtained is high and electric conductivity is excellent.
Detailed description of the invention
Fig. 1 is silicon carbide nanometer line-alginic acid fibre strength-strain figure made from the method for the present invention；
Fig. 2 is silicon carbide nanometer line-alginic acid fibre VA characteristic curve made from the method for the present invention；
Fig. 3 is silicon carbide nanometer line-alginic acid fibre scanning electron microscope (SEM) photo made from the method for the present invention；
Specific embodiment
Below with reference to embodiment, the present invention will be further described
Implementation of the invention is as follows:
Embodiment 1
Cotton shape silicon carbide nanometer line prepared by laboratory: being first placed in flask by step a, then with sulfuric acid and nitric acid
Mixed acid sufficiently reacts 6 hours under the conditions of 120 DEG C of temperature, and wherein the volume ratio of sulfuric acid and nitric acid is 3:1；Spend later from
Sub- water repeated flushing is filtered, is dried through the processed silicon carbide nanometer line of nitration mixture to neutrality.
Step b: deionized water, ammonium hydroxide and polyethylene glycol are added into the beaker for the silicon carbide nanometer line for filling drying
400, it is placed in 60 DEG C of baking oven and reacts 3 days, wherein the volume ratio of deionized water, ammonium hydroxide and polyethylene glycol 400 is 500:30:
3.Beaker is taken out from baking oven and is cooled to room temperature, filters and dries after being rinsed 3 times with deionized water, the silicon carbide weighed is received
Rice noodles prepare the silicon carbide nanometer line solution that mass fraction is 0.3%, spare.
Step c: first sodium alginate being added in deionized water, under room temperature after stirring swelling 2 hours, then under the conditions of 80 DEG C
The sodium alginate soln that mass fraction is 5% is prepared in stirring 3 hours.
Step d: the silicon carbide nanometer line solution being prepared is mixed with sodium alginate soln by the volume ratio of 2:1, is filled
After dividing stirring, pumps in the calcium chloride solution for being 5% with the injection rate implantation quality score of 100ml/min, obtain through digital injection
To gel state sodium alginate nanometer silicon carbide as-spun fibre.By the as-spun fibre being prepared naturally dry 6 hours at normal temperature,
Up to mechanical property, electric conductivity excellent silicon carbide nanometer line/alginic acid composite fibre.
The tensile strength of the present embodiment, the test process of electric conductivity are as follows: using universal testing machine to nanometer silicon carbide
Line-alginic acid composite fibre carries out extension test, is tested with the rate of extension of 5mm/min, and test fibre length is 7cm；
Using the resistance of four probe method measurement product, measurement voltage is 10V, fiber is connected between two probes, in hollow state
The lower measurement for carrying out resistance value.
Test result: true tensile strength and resistance value result are respectively 7.9N and 2.1 × 10-11Ω。
Embodiment 2
Step a, b, c is same as Example 1.
Step d: the silicon carbide nanometer line solution being prepared is mixed with sodium alginate soln by the volume ratio of 1:1, is filled
After dividing stirring, pumps in the calcium chloride solution for being 5% with the injection rate implantation quality score of 100ml/min, obtain through digital injection
To gel state sodium alginate silicon carbide nanometer line as-spun fibre.By the as-spun fibre being prepared, naturally dry 6 is small at normal temperature
When to get mechanical property, heating conduction and the excellent silicon carbide nanometer line/alginic acid composite fibre of electromagnetic shielding performance.
The tensile strength of the present embodiment, the test process of electric conductivity are as follows: using universal testing machine to nanometer silicon carbide
Line-alginic acid composite fibre carries out extension test, is tested with the rate of extension of 5mm/min, and test fibre length is 7cm；
Using the resistance of four probe method measurement product, measurement voltage is 10V, fiber is connected between two probes, in hollow state
The lower measurement for carrying out resistance value.
Test result: true tensile strength and resistance value result are respectively 4.7N and 1.1 × 10-11Ω。
Embodiment 3
Step a, b, c is same as Example 1.
Step d: the silicon carbide nanometer line solution being prepared is mixed with sodium alginate soln by the volume ratio of 1:1.2,
After being sufficiently stirred, pumped in the calcium chloride solution for being 5% with the injection rate implantation quality score of 100ml/min through digital injection,
Obtain gel state sodium alginate silicon carbide nanometer line composite fibre.By the as-spun fibre being prepared naturally dry 6 at normal temperature
Hour to get mechanical property, heating conduction and the excellent silicon carbide nanometer line/alginic acid composite fibre of electromagnetic shielding performance.
The tensile strength of the present embodiment, the test process of electric conductivity are as follows: using universal testing machine to nanometer silicon carbide
Line-alginic acid composite fibre carries out extension test, is tested with the rate of extension of 5mm/min, and test fibre length is 7cm；
Using the resistance of four probe method measurement product, measurement voltage is 10V, fiber is connected between two probes, in hollow state
The lower measurement for carrying out resistance value.
Test result: true tensile strength and resistance value result are respectively 6.2N and 8.8 × 10-12Ω。
Embodiment 4
Step a, b, c is same as Example 1.
Step d: the silicon carbide nanometer line solution being prepared is mixed with sodium alginate soln by the volume ratio of 1:1.5,
After being sufficiently stirred, pumped in the calcium chloride solution for being 5% with the injection rate implantation quality score of 100ml/min through digital injection,
Obtain gel state sodium alginate silicon carbide nanometer line as-spun fibre.By the as-spun fibre being prepared naturally dry 6 at normal temperature
Hour to get mechanical property, heating conduction and the excellent silicon carbide nanometer line/alginic acid composite fibre of electromagnetic shielding performance.
The tensile strength of the present embodiment, the test process of electric conductivity are as follows: using universal testing machine to nanometer silicon carbide
Line-alginic acid composite fibre carries out extension test, is tested with the rate of extension of 5mm/min, and test fibre length is 7cm；
Using the resistance of four probe method measurement product, measurement voltage is 10V, fiber is connected between two probes, in hollow state
The lower measurement for carrying out resistance value.
Test result: true tensile strength and resistance value result are respectively 6.4N and 7.1 × 10-12Ω。
Embodiment 5
Step a, b, c is same as Example 1.
Step d: the silicon carbide nanometer line solution being prepared is mixed with sodium alginate soln by the volume ratio of 1:2, is filled
After dividing stirring, pumps in the calcium chloride solution for being 5% with the injection rate implantation quality score of 100ml/min, obtain through digital injection
To gel state sodium alginate silicon carbide nanometer line as-spun fibre.By the as-spun fibre being prepared, naturally dry 6 is small at normal temperature
When to get mechanical property, heating conduction and the excellent silicon carbide nanometer line/alginic acid composite fibre of electromagnetic shielding performance.
The tensile strength of the present embodiment, the test process of electric conductivity are as follows: using universal testing machine to nanometer silicon carbide
Line-alginic acid composite fibre carries out extension test, is tested with the rate of extension of 5mm/min, and test fibre length is 7cm；
Using the resistance of four probe method measurement product, measurement voltage is 10V, fiber is connected between two probes, in hollow state
The lower measurement for carrying out resistance value.
Test result: true tensile strength and resistance value result are respectively 6.8N and 5.3 × 10-12Ω。
Comprehensive mechanical property and electric conductivity consider that preparation-obtained silicon carbide nanometer line-alginic acid is multiple in embodiment 3
The performance of condensating fiber is the most excellent, true tensile strength 6.2N, and resistance value is 8.8 × 10-12Ω。
Claims (7)
1. a kind of prepare silicon carbide nanometer line-alginic acid composite fibre spinning process, which comprises the steps of:
1) pretreatment of silicon carbide nanometer line: silicon carbide nanometer line is rinsed after mixed acid is handled with deionized water, is dried through filtering
Deionized water, ammonium hydroxide and polyethylene glycol 400 are added after dry to be placed in baking oven and react, then is configured to silicon carbide after filtering drying
Nanowire solution is spare；
2) it prepares sodium alginate soln: first sodium alginate being added in deionized water, stirring and dissolving, is then being heated at normal temperature
Under the conditions of be stirred up to required sodium alginate soln；
3) it prepares silicon carbide nanometer line/sodium alginate spinning solution: the pretreated silicon carbide nanometer line of step 1) is added to
To get required silicon carbide nanometer line/sodium alginate spinning solution in the sodium alginate soln that step 2) is prepared；
4) prepare silicon carbide nanometer line/alginic acid as-spun fibre: the spinning solution that step 3) is obtained is solidified through coagulating bath
Afterwards up to required silicon carbide nanometer line/alginic acid as-spun fibre；
5) prepare silicon carbide nanometer line/alginic acid composite fibre: the as-spun fibre that step 4) is obtained passes through after natural drying i.e.
Obtain required silicon carbide nanometer line/alginic acid composite fibre.
2. according to claim 1 prepare silicon carbide nanometer line/alginic acid composite fibre spinning process, feature exists
In in the step 1), mixed acid is the sulfuric acid and nitric acid of volume ratio 3:1；The body of deionized water, ammonium hydroxide and polyethylene glycol 400
Product is than being 500:30:3, and after deionized water, ammonium hydroxide and polyethylene glycol 400 are added, the mass fraction of silicon carbide nanometer line solution is
0.3%.
3. according to claim 1 prepare silicon carbide nanometer line/alginic acid composite fibre spinning process, feature exists
In in the step 2), the stirring at normal temperature time is 2 hours, 80-12 DEG C of heating stirring temperature, and mixing time is 1-3 hours, system
The mass fraction of standby obtained sodium alginate soln is 3-5%.
4. according to claim 1 prepare silicon carbide nanometer line/alginic acid composite fibre spinning process, feature exists
In in the step (3), the volume ratio of silicon carbide nanometer line solution and sodium alginate soln is 1:0.5-2.
5. according to claim 1 prepare silicon carbide nanometer line/alginic acid composite fibre spinning process, feature exists
In in the step (4), coagulating bath is the calcium chloride water that mass fraction is 5%.
6. according to claim 1 prepare silicon carbide nanometer line/alginic acid composite fibre spinning process, feature exists
In in the step (4), spinning solution temperature is 25 DEG C, and coagulation bath temperature is 20-35 DEG C.
7. according to claim 1 prepare silicon carbide nanometer line/alginic acid composite fibre spinning process, feature exists
In in the step (5), the naturally dry time is 3-8 hours.
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| CN201810812178.4A CN108950730B (en) | 2018-07-23 | 2018-07-23 | Spinning method for preparing silicon carbide nanowire/alginic acid composite fiber |
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