CN105369601A - Natural silk electric conduction fiber preparation method - Google Patents
Natural silk electric conduction fiber preparation method Download PDFInfo
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- CN105369601A CN105369601A CN201410406972.0A CN201410406972A CN105369601A CN 105369601 A CN105369601 A CN 105369601A CN 201410406972 A CN201410406972 A CN 201410406972A CN 105369601 A CN105369601 A CN 105369601A
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Abstract
The present invention relates to a natural silk electric conduction fiber preparation method, wherein natural silk fibers are adopted as a raw material, a chemical silver plating method is used, and the silver plating process is adjusted to improve the silver plating layer uniformity and the binding fastness between the silver plating layer and the matrix fibers. According to the present invention, the method has characteristics of simple operation, stable process performance, less energy consumption, and easy industrial production; and the electric conduction fibers prepared by using the method have characteristics of high plating layer binding fastness, good electric conduction performance and retaining of characteristics of original fibers, and can be adopted as the electric conduction fibers for a variety of textiles, wherein the specific surface resistance achieves 3-10 omega/cm.
Description
Technical field
the present invention relates to a kind of preparation method of conductive fiber, particularly a kind of preparation method of real silk conductive fiber.The method, by making real silk have good electric conductivity at real silk coating surface layer of metal silverskin, belongs to new textile material field.
Background technology
silver plated fiber is a kind of high performance functional fibre, and the function such as the antibacterial and deodouring of its uniqueness, anti-electromagnetic radiation, antistatic, regulate body temperature is attracted attention by people.The outer plating technology of fiber mainly contains chemical plating, plating and Vacuum Deposition three class.Adopt Electroless Silver Plating have technique simple, be applicable to the advantages such as irregular matrix material, cost are lower, but it is difficult to there is reaction in current Electroless Silver Plating, control bath stability is poor, and silver-plated price is more expensive, the conductive fiber coating problem that not evenly binding strength is not high of preparation.
before making the present invention, Chinese invention patent, CNl311369A, disclose a kind of chemical silver plating method of organic fiber, take silver ammino solution as silver plating liquid, before silver-plated, raw material is cleaned in acetone soln, then surface activation process is carried out, catalyst P dCl2 catalysis with salpeter solution and hydrochloric acid solution.The method use this organic solvent of acetone, have employed again precious metal palladium as catalyst, cost compare is high.Chinese invention patent CN100570047C discloses a kind of preparation method of high-performance conductive fiber, using sodium potassium tartrate tetrahydrate as reductant, adopts oxalic acid solution to soak solidification.Have employed organic solvent 2-dichloroethanes or dimethylbenzene equally as alligatoring agent, cost compare is high.Chinese invention patent CN101012552A discloses a kind of stable fibre chemistry silver-coating method that can repeatedly supplement, and using formaldehyde as reductant, has reacted rear interpolation ammoniacal liquor and formaldehyde, continues chemical silvering.Formaldehyde toxic and volatile, adopts formaldehyde to pollute.
Summary of the invention
Problem to be solved by this invention is the deficiency overcoming prior art existence, provides a kind of preparation method of real silk conductive fiber.
The technical solution adopted in the present invention is:
a kind of preparation method of real silk conductive fiber, take cocoon fiber as raw material, it is characterized in that, comprise the steps: to come unstuck to silk fiber, sensitization pre-treatment, adds low concentration silver nitrate-ammonia spirit activation, then carries out chemical silvering, add chelating ligands agent when chemical silvering and replace partial ammonia water, after silver-plated, carry out hot setting process.
preferably, described sensitization pre-treatment, floods 10 ~ 20min under adopting the stannous chloride solution normal temperature of 1 ~ 20g/L, and the cocoon fiber after then adopting the sodium bicarbonate solution of 1g/L to rinse stannous chloride dipping, clarifies to cleaning solution.
preferably, after described silver ammino solution activation, the formula carrying out chemical plating liquid is composed as follows:
reducing solution is filled a prescription: glucose: 3 ~ 10g/L;
oxidation solution is filled a prescription: silver nitrate 5 ~ 30g/L; Ammoniacal liquor: appropriate; Chelating ligands agent 0.01 ~ 2g/L.
preferably, the chelating ligands agent added in described chemical silvering is nitrilotriacetic acid salt, citrate or pyrophosphate.
preferably, described silver-plated after carry out hot setting process, hot setting is temperature is 90 ~ 150 DEG C, time 4 ~ 8min.
The principle of foundation of the present invention is:
general when carrying out sensitized treatment with stannous chloride, not very even, easily washed, this patent adds sodium bicarbonate solution cleaning, and solution ph is raised, and stannous chloride forms nanogel and is deposited on fiber surface, formed relatively more firm, more uniform sedimentary deposit.Thereafter adopt the activation of low concentration silver ammino solution, strengthen the adhesion of matrix and silver, make silver-plated after be not easy to fall down.Chemistry crosses in formula of liquid and adds chelating ligands agent, for stable plating solution, reduces surface porosity factor and roughness, makes coating surface even.The Ag particle of separating out is less, forms nano-Ag particles, can anti-oxidation, reduces the impurity that coating is separated out, and increases the uniformity that Argent grain is separated out.
compared with prior art, the present invention has following obvious advantage:
form the nano-colloid of tin ash during sodium bicarbonate cleaning stannous chloride, Nano silver deposition can be helped even.Add chelating ligands agent in plating solution, the uniformity of coating and the binding strength between itself and matrix fiber can be significantly improved.The present invention is simple to operate on the whole, and processing performance is stablized, and cost is low, and power consumption is few, is easy to suitability for industrialized production.Adopt conductive fiber prepared by the present invention, coating binding strength is high, and electric conductivity is good, and specific area resistance reaches 3 ~ 10 Ω/cm, and retains the characteristic of original cocoon fiber, can use in multiple textile material.
Detailed description of the invention
below in conjunction with embodiment, technical solution of the present invention and effect are further described.
embodiment 1:
the present embodiment adopts 1g real silk fabric to be raw material.
the first step: come unstuck.Join in the deionized water of 50mL by 0.025g sodium carbonate, bath temperature is 95 ° of C, stirs.After add load weighted real silk fabric (1g) and stir 30min.Abundant washing.Repeat once.
second step: sensitization.Weighing 0.05g stannous chloride is dissolved in 0.05mL hydrochloric acid, and join in 50mL deionized water until completely dissolved again, the real silk fabric finally adding previous step process fully stirs 10min, and temperature is 30 DEG C.The complete rear 1g/L sodium bicarbonate solution of sensitization embathes 3min, more fully washes.
tri-Walk: activation.Take 0.05g silver nitrate to be dissolved in a small amount of deionized water, then drip ammoniacal liquor in solution.There is reddish brown precipitation in solution during beginning, continue to drip ammoniacal liquor to solution clarification.Then add deionized water to 50mL, the cocoon fiber finally adding previous step process fully stirs 3min, and bath temperature is 30 DEG C. and fully washing is clean afterwards.4th step: deposition of silver.
1,112mL reducing solution is prepared: weigh 0.9g glucose and be fully dissolved in 112mL deionized water.
2,38mL silver liquid ammonia is prepared: weigh 0.5g silver nitrate and be dissolved in a small amount of deionized water, then drip ammoniacal liquor in solution.There is precipitation during beginning, continue to drip ammoniacal liquor and clarify to solution.Add deionized water again to 37.5mL, finally add 0.002g nitrilotriacetic acid sodium and be dissolved in wherein.
3, the silver liquid ammonia prepared is poured in reducing solution, shake up.Add rapidly the cocoon fiber that the 3rd step activates, 30 DEG C of beginnings are silver-plated, insulation 2min, then with the ramp to 50 of 1 DEG C per minute DEG C insulation 30min.
5th step: solidification.Take out fabric, bake 8 minutes at 150 DEG C, washing, 80 DEG C of oven dry, obtain conduction real silk fabric.
test shows, the conduction real silk fabric electric conductivity of preparation is good, and sheet resistance is 2-8 Ω/cm, remains the characteristic of original fiber, soft.
embodiment 2:
the present embodiment adopts 1g real silk fabric to be raw material.
the first step: come unstuck.Join in the deionized water of 50mL by 0.03g sodium carbonate, bath temperature is 98 ° of C, stirs.After add load weighted real silk fabric (1g) and stir 32min.Abundant washing.Repeat once.
second step: sensitization.Weighing 0.06g stannous chloride is dissolved in 0.05mL hydrochloric acid, and join in 50mL deionized water until completely dissolved again, the real silk fabric finally adding previous step process fully stirs 20min, and temperature is 25 DEG C.The complete rear 1g/L sodium bicarbonate solution of sensitization embathes 5min, more fully washes.
tri-Walk: activation.Take 0.04g silver nitrate to be dissolved in a small amount of deionized water, then drip ammoniacal liquor in solution.There is reddish brown precipitation in solution during beginning, continue to drip ammoniacal liquor to solution clarification.Then add deionized water to 50mL, the cocoon fiber finally adding previous step process fully stirs 5min, and bath temperature is 25 DEG C. and fully washing is clean afterwards.4th step: deposition of silver.
1,112mL reducing solution is prepared: weigh 0.9g glucose and be fully dissolved in 112mL deionized water.
2,38mL silver liquid ammonia is prepared: weigh 0.6g silver nitrate and be dissolved in a small amount of deionized water, then drip ammoniacal liquor in solution.There is precipitation during beginning, continue to drip ammoniacal liquor and clarify to solution.Add deionized water again to 37.5mL, finally add 0.003g nitrilotriacetic acid sodium and be dissolved in wherein.
3, the silver liquid ammonia prepared is poured in reducing solution, shake up.Add rapidly the cocoon fiber that the 3rd step activates, 32 DEG C of beginnings are silver-plated, insulation 5min, then with the ramp to 50 of 1 DEG C per minute DEG C insulation 30min.
5th step: solidification.Take out real silk fabric, bake 6 minutes at 120 DEG C, washing, then 80 DEG C of oven dry, obtain conduction real silk fabric.
test shows, the conduction real silk fabric electric conductivity of preparation is good, and sheet resistance is 4-8 Ω/cm, remains the characteristic of original fiber, soft.
embodiment 3:
the present embodiment adopts 1g real silk fabric to be raw material.
the first step: come unstuck.Join in the deionized water of 50mL by 0.028g sodium carbonate, bath temperature is 97 ° of C, stirs.After add load weighted real silk fabric (1g) and stir 35min.Abundant washing.Repeat once.
second step: sensitization.Weighing 0.04g stannous chloride is dissolved in 0.05mL hydrochloric acid, and join in 50mL deionized water until completely dissolved again, the real silk fabric finally adding previous step process fully stirs 15min, and temperature is 30 DEG C.The complete rear 1g/L sodium bicarbonate solution of sensitization embathes 5min, more fully washes.
tri-Walk: activation.Take 0.03g silver nitrate to be dissolved in a small amount of deionized water, then drip ammoniacal liquor in solution.There is reddish brown precipitation in solution during beginning, continue to drip ammoniacal liquor to solution clarification.Then add deionized water to 50mL, the cocoon fiber finally adding previous step process fully stirs 5min, and bath temperature is 35 DEG C. and fully washing is clean afterwards.
4th step: deposition of silver.
1,112mL reducing solution is prepared: weigh 1.0g glucose and be fully dissolved in 112mL deionized water.
2,38mL silver liquid ammonia is prepared: weigh 0.7g silver nitrate and be dissolved in a small amount of deionized water, then drip ammoniacal liquor in solution.There is precipitation during beginning, continue to drip ammoniacal liquor and clarify to solution.Add deionized water again to 37.5mL, finally add 0.004g sodium pyrophosphate and be dissolved in wherein.
3, the silver liquid ammonia prepared is poured in reducing solution, shake up.Add rapidly the cocoon fiber that the 3rd step activates, 32 DEG C of beginnings are silver-plated, insulation 10min, then with the ramp to 50 of 2 DEG C per minute DEG C insulation 20min.
5th step: solidification.Take out real silk fabric, bake 8 minutes at 130 DEG C, washing, then 85 DEG C of oven dry, obtain conduction real silk fabric.
test shows, the conduction real silk fabric electric conductivity of preparation is good, and sheet resistance is 5-8 Ω/cm, remains the characteristic of original fiber, soft.
Claims (5)
1. the preparation method of a real silk conductive fiber, take cocoon fiber as raw material, it is characterized in that, comprise the steps: to come unstuck to cocoon fiber, sensitization pre-treatment, adds low concentration silver nitrate-ammonia spirit activation, then carries out chemical silvering, add chelating ligands agent when chemical silvering and replace partial ammonia water, after silver-plated, carry out hot setting process.
2. the preparation method of a kind of real silk conductive fiber according to claim 1, it is characterized in that, described sensitization pre-treatment, 10 ~ 20min is flooded under adopting the stannous chloride solution normal temperature of 1 ~ 20g/L, then the cocoon fiber after adopting the sodium bicarbonate solution of 1g/L to rinse stannous chloride dipping, clarifies to cleaning solution.
3. the preparation method of a kind of real silk conductive fiber according to claim 1, is characterized in that, after described silver ammino solution activation, the formula carrying out chemical plating liquid is composed as follows:
Reducing solution is filled a prescription: glucose: 3 ~ 10g/L;
Oxidation solution is filled a prescription: silver nitrate 5 ~ 30g/L; Ammoniacal liquor: appropriate; Chelating ligands agent 0.01 ~ 2g/L.
4. the preparation method of a kind of real silk conductive fiber according to claim 3, is characterized in that, the chelating ligands agent added in described chemical silvering is nitrilotriacetic acid salt, citrate or pyrophosphate.
5. the preparation method of a kind of real silk conductive fiber according to claim 1, is characterized in that, described silver-plated after carry out hot setting process, hot setting is temperature is 90 ~ 150 DEG C, time 4 ~ 8min.
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| CN201410406972.0A CN105369601A (en) | 2014-08-19 | 2014-08-19 | Natural silk electric conduction fiber preparation method |
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| CN201410406972.0A CN105369601A (en) | 2014-08-19 | 2014-08-19 | Natural silk electric conduction fiber preparation method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012552A (en) * | 2007-01-27 | 2007-08-08 | 吕琳 | Steady multitime supplementary fiber chemical silver coating method |
| CN102899890A (en) * | 2012-10-31 | 2013-01-30 | 昆明理工大学 | Aramid fiber surface metallization treatment method |
| CN102936835A (en) * | 2012-12-05 | 2013-02-20 | 苏州大学 | Preparation method of nano-silver antibacterial real silk |
| CN103194891A (en) * | 2013-03-31 | 2013-07-10 | 卜庆革 | Silver-based anti-bacterial and anti-static fibers, production method of fibers, and clothes made from fibers |
| CN103668944A (en) * | 2013-12-16 | 2014-03-26 | 天诺光电材料股份有限公司 | Silvered aramid conductive fiber and preparation method thereof |
-
2014
- 2014-08-19 CN CN201410406972.0A patent/CN105369601A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012552A (en) * | 2007-01-27 | 2007-08-08 | 吕琳 | Steady multitime supplementary fiber chemical silver coating method |
| CN102899890A (en) * | 2012-10-31 | 2013-01-30 | 昆明理工大学 | Aramid fiber surface metallization treatment method |
| CN102936835A (en) * | 2012-12-05 | 2013-02-20 | 苏州大学 | Preparation method of nano-silver antibacterial real silk |
| CN103194891A (en) * | 2013-03-31 | 2013-07-10 | 卜庆革 | Silver-based anti-bacterial and anti-static fibers, production method of fibers, and clothes made from fibers |
| CN103668944A (en) * | 2013-12-16 | 2014-03-26 | 天诺光电材料股份有限公司 | Silvered aramid conductive fiber and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王政: ""导电弹性纤维的研制"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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Application publication date: 20160302 |