CN101871138A - Method for manufacturing nylon6/nanometer SiO2 composite fiber material - Google Patents
Method for manufacturing nylon6/nanometer SiO2 composite fiber material Download PDFInfo
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- CN101871138A CN101871138A CN 201010230835 CN201010230835A CN101871138A CN 101871138 A CN101871138 A CN 101871138A CN 201010230835 CN201010230835 CN 201010230835 CN 201010230835 A CN201010230835 A CN 201010230835A CN 101871138 A CN101871138 A CN 101871138A
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- sio
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Abstract
The invention discloses a method for manufacturing an nylon6/nanometer SiO2 composite fiber material, which comprises the following steps: adopting no-soap emulsion polymerization process to modify the surface of the nanometer SiO2 so as to enable the surface of the nanometer SiO2 grains to be attached with a layer of polymer film having good compatibility with the nylon6 polymer molecules to obtain the modified nanometer SiO2 powder; slicing, mixing, evenly stirring the modified nanometer SiO2 powder and the nylon6; carrying out melting and extruding processes to prepare into composite material pellet slices; and using a composite spinning machine to carry out melting and spinning on the nylon6/SiO2 composite material pellet slices to prepare the nylon6/nanometer SiO2 composite fiber material. In the invention, the prepared modified nanometer SiO2/nylon6 has high compatibility; the nylon6/SiO2 composite material is prepared by the steps of melting, extruding, cooling, pelleting and melting and spinning; and the method has simple processing, does not influence the polymerization of nylon, ensures the production efficiency, and ensures the component uniformity and performance stability of the formed composite fiber materials.
Description
Technical field
The invention belongs to nylon 6 modified fiber materials of polymer composite, i.e. nylon 6/ nanometer SiO
2The complex fiber material preparation method.
Technical background
Nylon 6 has excellent comprehensive performances, but because have that water absorption rate is big, heat distortion temperature is low, strong alkali-acid resistance is poor, dry state and low temperature impact strength is low and shortcoming such as easy firing, thereby influence the DIMENSIONAL STABILITY and the electrical property of goods.Since people such as Japanese Y.Fukushima in 1987 adopted in-situ inserted complex method to prepare nylon 6/ Nano composite material of montmorillonite first, lot of domestic and international researcher had done a large amount of work on the study on the modification of nylon 6, nanometer SiO
2With the compound of nylon 6 be one of its method of modifying, up to the present, the main practice both domestic and external is to adopt wet-treating nanometer SiO
2, be about to nanometer SiO
2Treatment fluid joins in the caprolactam, makes nylon 6/ nanometer SiO by the original position ring-opening polymerization again
2Complex fiber material, just nylon 6/ nanometer SiO
2The complex fiber material preparation process is at nanometer SiO
2Nylon 6/poly compound forming process under the dispersity.This method advantage is polymer fiber material component homogeneous, the stable performance that forms, and its shortcoming is because SiO
2Adopt wet-treating, make that polymerization system polymerisation decrease in efficiency is that production efficiency descends.
Summary of the invention
In order to overcome wet-treating nanometer SiO
2Make nylon 6/ nanometer SiO
2The inefficient shortcoming of complex fiber material explained hereafter the present invention proposes a kind of nylon 6/ nanometer SiO
2The new method that complex fiber material is made.
This nylon 6/ nanometer SiO
2The complex fiber material preparation method is characterized in that, adopts the emulsifier-free emulsion polymerization method to nanometer SiO
2Carry out surface modification, make nanometer SiO
2Particle surface is enclosed one deck and the good polymer film of nylon 6/poly adduct molecule compatibility, gets modified Nano SiO
2Powder is beneficial to nanometer SiO
2Disperse, with modified Nano SiO
2Powder and nylon 6 slice mix, mix thoroughly, make it to become composite grain sheet by fusion, expressing technique again, with composite spinning machine with nylon 6/SiO
2Composite grain sheet carries out melt spinning, makes nylon 6/ nanometer SiO
2Complex fiber material.
Above-mentioned nylon 6/ nanometer SiO
2The complex fiber material preparation method, concrete steps are as follows:
One, modified Nano SiO
2The preparation of powder:
Weight ratio by following material is prepared:
1. nanometer SiO
2, 30-80nm 90-110 part
2. deionized water 900-1100 part
3. alpha-methylmercapto acrylic acid is 1.0～1.5 parts
4. acrylic acid is 1.0～1.5 parts
5. potassium peroxydisulfate is 0.01～0.015 part
Press following technological operation:
With 90-110 part nanometer SiO
2Put into reaction bulb with 2900-1100 part deionized water, move into ultrasonic dispersion 20min in the ultrasonic disperser, add 1.0～1.5 parts of α-Jia Jibingxisuans, 1.0～1.5 parts of acrylic acid and 0.01～0.015 part of potassium peroxydisulfate after above-mentioned suspension system being moved to Water Tank with Temp.-controlled again, stir, heat up, under 70-90 ℃ of temperature, react 2-4h, after centrifugation, vacuumize makes modified Nano SiO to constant weight
2Powder.
Two, nylon 6/ nanometer SiO
2The preparation of composite grain sheet:
Weight ratio by following material is prepared:
1. nylon 6 slice 90-110 part
2. modified Nano SiO
21～5 part in powder
Press following technological operation:
With 90-110 part nylon 6 slice and modified Nano SiO
21～5 part of mixing, mix thoroughly after, melt extrude through double screw extruder, melt temperature 270-290 ℃, cooling, granulation make nylon 6/SiO
2Composite grain sheet.
Three, with composite spinning machine with above-mentioned nylon 6/SiO
2Composite grain sheet carries out melt spinning, and spinning temperature 270-290 ℃, spray silk machine aperture 0.8-1.2mm, spinning speed 50-150m/min, silk hot-stretch under 80-100 ℃ of environment just, 130-170 ℃ is carried out HEAT SETTING, obtains nylon 6/SiO
2The composite fiber product.On the Instron1122 universal testing machine, measure fibrous mechanical property.
In the method for the present invention, the modified Nano SiO that adopts the emulsifier-free emulsion polymerization method to make
2Have the compatibility of height with nylon 6, by fusion, extrude, cooling, granulation, melt spinning, make nylon 6/SiO
2Complex fiber material, technical process is simple, and does not influence the polymerisation of nylon, has both protected and has levied production efficiency, has guaranteed the homogeneous of composite fibre material component and the stablizing of performance that form simultaneously again.
The specific embodiment
Under to enumerate 2 example in detail as follows:
Example 1:
One, with 100 parts of nanometer SiO
2Put into reaction bulb with 1100 parts of deionized waters, move into and disperse 20min in the ultrasonic disperser, again above-mentioned suspension system is moved in Huan's warm water tank, add 1.5 parts of α-Jia Jibingxisuans, 1.0 parts of acrylic acid and 0.012 part of potassium peroxydisulfate then, stir, heat up, under 85 ℃ of temperature, react 3h, after centrifugation, vacuumize makes modified Nano SiO to constant weight
2Powder.
Two, with 100 parts of nylon 6 slices and 3 parts of modified Nano SiO
2Powder, mix thoroughly after, under 280 ℃ of temperature, melt extrude, through the cooling, granulation, make nylon 6/SiO
2Composite grain sheet.
Three, this sheet is carried out melt spinning, 280 ℃ of spinning temperatures, spinning speed 100m/min, silk hot-stretch under 90 ℃ of environment just, 150 ℃ are carried out HEAT SETTING, obtain fiber product.This product sample is measured on the Instro1122 universal testing machine, and its fracture strength is 7.8cN.dtex
-1, elongation at break 25.7%, initial modulus are 63.1cN.dtex
-1
Example 2
One, with 90 fens nanometer SiO
2Put into reaction bulb with 1000 parts of deionized waters, move into and disperse 20min in the ultrasonic disperser, again above-mentioned suspension system is moved in Huan's warm water tank, add 1.5 parts of α-Jia Jibingxisuans, 1.5 acrylic acid and 0.015 part of potassium peroxydisulfate then, stir, heat up, under 90 ℃ of temperature, react 2h, be dried to constant weight, make modified Nano SiO through the centrifugation final vacuum
2Powder.
Two, with 110 parts of nylon 6 slices and 3 parts of modified Nano SiO
2Powder, mix thoroughly after, under 280 ℃ of temperature, melt extrude, through the cooling, granulation, make nylon 6/SiO
2Composite grain sheet.
Three, this sheet is carried out melt spinning, spinning condition is identical with example 1, obtains fiber product.This product sample is measured on the Instron1122 universal testing machine, and its fracture strength, elongation at break, initial modulus are respectively 7.5cN.dtex
-1, 23.5%, 57.8cN.dtex
-1
Claims (4)
1. nylon 6/ nanometer SiO
2The complex fiber material preparation method is characterized in that, adopts the emulsifier-free emulsion polymerization method to nanometer SiO
2Carry out surface modification, make nanometer SiO
2Particle surface is enclosed one deck and the good polymer film of nylon 6/poly adduct molecule compatibility, gets modified Nano SiO
2Powder is beneficial to nanometer SiO
2Disperse, with modified Nano SiO
2Powder and nylon 6 slice mix, mix thoroughly, make it to become composite grain sheet by fusion, expressing technique again, with composite spinning machine with nylon 6/SiO
2Composite grain sheet carries out melt spinning, makes nylon 6/ nanometer SiO
2Complex fiber material.
2. nylon 6/ nanometer SiO according to claim 1
2The complex fiber material preparation method is characterized in that, modified Nano SiO
2The preparation method of powder is as follows:
Weight ratio by following material is prepared:
1. nanometer SiO
2, 30-80nm 90-110 part
2. deionized water 900-1100 part
3. alpha-methylmercapto acrylic acid is 1.0～1.5 parts
4. acrylic acid is 1.0～1.5 parts
5. potassium peroxydisulfate is 0.01～0.015 part
Press following technological operation:
With 90-110 part nanometer SiO
2Put into reaction bulb with 2900-1100 part deionized water, move into ultrasonic dispersion 20min in the ultrasonic disperser, add 1.0～1.5 parts of α-Jia Jibingxisuans, 1.0～1.5 parts of acrylic acid and 0.01～0.015 part of potassium peroxydisulfate after above-mentioned suspension system being moved to Water Tank with Temp.-controlled again, stir, heat up, under 70-90 ℃ of temperature, react 2-4h, after centrifugation, vacuumize makes modified Nano SiO to constant weight
2Powder.
3. nylon 6/ nanometer SiO according to claim 1
2The complex fiber material preparation method is characterized in that, nylon 6/ nanometer SiO
2The preparation method of composite grain sheet is as follows:
Weight ratio by following material is prepared:
1. nylon 6 slice 90-110 part
2. modified Nano SiO
21～5 part in powder
Press following technological operation:
With 90-110 part nylon 6 slice and modified Nano SiO
21～5 part of mixing, mix thoroughly after, melt extrude through double screw extruder, melt temperature 270-290 ℃, cooling, granulation make nylon 6/SiO
2Composite grain sheet.
4. nylon 6/ nanometer SiO according to claim 1
2The complex fiber material preparation method is characterized in that, with composite spinning machine with nylon 6/SiO
2Composite grain sheet carries out melt spinning, and spinning temperature 270-290 ℃, spray silk machine aperture 0.8-1.2mm, spinning speed 50-150m/min, silk hot-stretch under 80-100 ℃ of environment just, 130-170 ℃ is carried out HEAT SETTING, obtains nylon 6/SiO
2The composite fiber product.
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| CN 201010230835 CN101871138A (en) | 2010-07-14 | 2010-07-14 | Method for manufacturing nylon6/nanometer SiO2 composite fiber material |
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|---|---|---|---|
| CN 201010230835 CN101871138A (en) | 2010-07-14 | 2010-07-14 | Method for manufacturing nylon6/nanometer SiO2 composite fiber material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746715A (en) * | 2012-05-24 | 2012-10-24 | 北京化工大学 | Silica with surface subjected to polymerization modification, and preparation method thereof |
| CN103290510A (en) * | 2013-05-24 | 2013-09-11 | 宁波三邦日用品有限公司 | Far infrared polypropylene-polyamide composite superfine fiber and production method thereof |
| CN104356640A (en) * | 2014-11-11 | 2015-02-18 | 河北工业大学 | Preparation method of polyacrylate compound particles for nylon 6 low-temperature toughening modification |
| CN106192071A (en) * | 2016-08-17 | 2016-12-07 | 江苏鸿顺合纤科技有限公司 | A kind of preparation method of the composite fibre with binding function |
| CN106400171A (en) * | 2016-08-31 | 2017-02-15 | 安徽东锦服饰有限公司 | Preparation method of fiber forming composite material with permeability |
| WO2017088199A1 (en) * | 2015-11-24 | 2017-06-01 | 南通新帝克单丝科技股份有限公司 | Nano-modified large-diameter copolymerized polyamide monofilament and production method therefor |
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| JP2002008913A (en) * | 2000-06-19 | 2002-01-11 | Daido Electronics Co Ltd | Rare earth magnet and its molding material |
| CN1357650A (en) * | 2000-12-07 | 2002-07-10 | 天津市发博纺织材料有限责任公司 | Jinlun-6 uvioresistant fiber and its production process |
| CN101215416A (en) * | 2007-12-26 | 2008-07-09 | 华东理工大学 | Method for preparing nano silicon dioxide/polycaprolactam composite resin |
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2010
- 2010-07-14 CN CN 201010230835 patent/CN101871138A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002008913A (en) * | 2000-06-19 | 2002-01-11 | Daido Electronics Co Ltd | Rare earth magnet and its molding material |
| CN1357650A (en) * | 2000-12-07 | 2002-07-10 | 天津市发博纺织材料有限责任公司 | Jinlun-6 uvioresistant fiber and its production process |
| CN101215416A (en) * | 2007-12-26 | 2008-07-09 | 华东理工大学 | Method for preparing nano silicon dioxide/polycaprolactam composite resin |
Non-Patent Citations (1)
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746715A (en) * | 2012-05-24 | 2012-10-24 | 北京化工大学 | Silica with surface subjected to polymerization modification, and preparation method thereof |
| CN103290510A (en) * | 2013-05-24 | 2013-09-11 | 宁波三邦日用品有限公司 | Far infrared polypropylene-polyamide composite superfine fiber and production method thereof |
| CN103290510B (en) * | 2013-05-24 | 2015-07-15 | 宁波三邦日用品有限公司 | Far infrared polypropylene-polyamide composite superfine fiber and production method thereof |
| CN104356640A (en) * | 2014-11-11 | 2015-02-18 | 河北工业大学 | Preparation method of polyacrylate compound particles for nylon 6 low-temperature toughening modification |
| CN104356640B (en) * | 2014-11-11 | 2016-05-11 | 河北工业大学 | The preparation method of polyacrylate compound particle for nylon 6 low temperature toughening modifyings |
| WO2017088199A1 (en) * | 2015-11-24 | 2017-06-01 | 南通新帝克单丝科技股份有限公司 | Nano-modified large-diameter copolymerized polyamide monofilament and production method therefor |
| CN106192071A (en) * | 2016-08-17 | 2016-12-07 | 江苏鸿顺合纤科技有限公司 | A kind of preparation method of the composite fibre with binding function |
| CN106400171A (en) * | 2016-08-31 | 2017-02-15 | 安徽东锦服饰有限公司 | Preparation method of fiber forming composite material with permeability |
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Open date: 20101027 |