CN102618958A - Production method of attapulgite modified phase-change air-conditioning nylon-6 - Google Patents
Production method of attapulgite modified phase-change air-conditioning nylon-6 Download PDFInfo
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- CN102618958A CN102618958A CN2012100799941A CN201210079994A CN102618958A CN 102618958 A CN102618958 A CN 102618958A CN 2012100799941 A CN2012100799941 A CN 2012100799941A CN 201210079994 A CN201210079994 A CN 201210079994A CN 102618958 A CN102618958 A CN 102618958A
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Abstract
The invention discloses a production method of attapulgite modified phase-change air-conditioning nylon-6, which includes: mixing one of organic phase change materials, namely paraffin, fatty acid and polyalcohol, with attapulgite; adding the mixture into polycaprolactam resin for fiber forming to make modified master-batches; mixing the master-batches with slices of the polycaprolactam resin; and obtaining the attapulgite modified phase-change air-conditioning nylon-6 by screw extrusion melting, spinning, drawing and winding processes. The modified maser-batches comprise, in weight percentage, 1-10% of the organic phase change materials, 30-60% of the attapulgite, 20-60% of the polycaprolactam resin, and 1-10% of additives. Mass mixture ratio of the master-batches to the slices of the polycaprolactam resin is 15-25:75-85. The nylon-6 produced by the method is fine in thermal storage and thermal regulation performances and physical and mechanical properties, the phase change materials are less apt to leak, no additional new equipment is needed in production, the process is simple, and the technique is mature and reliable.
Description
Technical field
The present invention relates to a kind of production method of phase-changing and temperature-regulating polyamide fibre 6, particularly a kind of production method of attapulgite modified polyamide fibre 6 belongs to polyamide fibre 6 spining technology fields.
Technical background
Phase-change material PCMs (phase change materials) is a kind of chemical material that utilizes latent heat of phase change to come energy storage and exoergic.That most of materials generally have is solid-state, liquid state and steam state three-phase; Different according to environment temperature; The phase of material can the phase co-conversion, and the phase deformation type generally can be divided into four types: the transformation mutually of solid-state-solid-state, solid-state-liquid state, liquid state-steam state, solid-state-steam state can take place.In the phase transition process, material absorbs heat or in environment, emits heat from environment, and the temperature of material remains unchanged.Generally speaking, the phase transition process latent heat of phase change of above-mentioned four kinds of forms increases gradually.Because back two kinds of phase transformation modes in phase transition process, are attended by the existence of a large amount of gases, material volume is changed greatly.Therefore, although their enthalpy of phase change are bigger, in reality, seldom use, what textiles was commonly used is the solid-liquid phase change material, and solid-solid phase transition material is also used to some extent.
Phase-change material of a great variety generally is divided into inorganic and organic two big types.Mineral-type mainly comprises some hydrate salts such as sulfate hydrate and nitrate hydrate or the like.Organic material mainly is paraffin, aliphatic acid and polyalcohol etc.
Intelligent temperature-regulation fabric is that phase-change material is applied to textiles; Utilize that phase-change material can absorb or discharge great amount of heat in the phase transition process; But can make simultaneously temperature keep constant characteristics,, make human body be in comfortable temperature range to keep the temperature substantially constant in the microclimate between human body and clothes; Thereby can prevent heat stress, and can under extreme environmental conditions, satisfy the needs of human body comfort.At present phase-change material is used for the method that textiles prepares the phase transformation intelligent temperature-regulation fabric and mainly contains four kinds: textile finishing method, microcapsules facture, spin processes, doughnut dipping completion method.
When utilizing spin processes to prepare the phase-changing and temperature-regulating fiber, in the melt or solution that phase-change material are added to the spinning poly compound, carry out spinning process then, with phase change material such as paraffin spinning at fibrous inside, thereby obtain containing the phase-changing and temperature-regulating fiber of phase change material.When adopting spin processes to produce phase change fiber, phase-change material can adopt microencapsulation form, also can adopt the polymeric phase change material of non-microencapsulation form, or employing is grafted to phase-change material on the high polymer.The phase change fiber that utilizes spin processes to produce, because phase-change material is evenly distributed on fibrous inside, phase-change material is difficult for revealing, so thermoregulation effect durability and washing durability are good.
Attapulgite is the natural nano structure mineral material with nanochannel structure, because they have very large specific area, adsorptivity is excellent; In addition, the attapulgite light specific gravity, Heat stability is good, cheap, also have very strong sterilization, deodorizing, detoxification, killing ability, have higher wholesomeness.
Polyamide fibre 6 (chemical name: capron(e)) have fracture strength height, excellent in abrasion resistance, light specific gravity, elasticity and good hygroscopicity, chemical stability good, be difficult for characteristics such as mould moth; Of many uses, can be used for making socks, underwear, garment material, non-weaving cloth etc.Along with the market competition aggravation, develop differential, functional nylon-6 fiber, improve added value of product, more and more important to improving the business economic benefit.
Summary of the invention
The invention provides a kind of production method of attapulgite modified phase-changing and temperature-regulating polyamide fibre 6, prepared polyamide fibre 6 not only has good physical and mechanical properties, and has good heat-accumulation temperature-adjustment characteristic.
1. the preparation method of attapulgite master batch
Earlier organic phase change material is carried out abundant mixing and absorption with attapulgite; Carry out the mixed modified master batch that gets with becoming fibre with the polycaprolactam polyimide resin again; The phase-change material percentage by weight is 10～20% in the modified master batch; The attapulgite percentage by weight is 30～60%, and polycaprolactam weight resin percentage is 20～60%, and weight of additive percentage is 5～15%.Described organic phase change material is a kind of in paraffin, aliphatic acid, the polyalcohol.Described attapulgite belongs to the inorganic particulate of the bar-shaped porous of nanoscale.The attapulgite microstructure is shown in accompanying drawing 1.
2. the preparation of attapulgite modified phase-changing and temperature-regulating polyamide fibre 6
Modified master batch is carried out blend with becoming fibre with the polycaprolactam resin slicer through the metering mixing; Mixed proportion is 15～25: 75～85, and in screw extruder, carrying out high temperature melt is the molten state spinning melt, and extruder temperature is 240～270 ℃; Fully mix in course of conveying through after the static mixing; Be injected into strand through filament spinning component again, spinning temperature is 240～270 ℃, and strand is 20 ± 5 ℃ through temperature; Humidity is 80 ± 5%, and wind speed is that the air-conditioning wind of 0.3～0.4 ℃ constant temperature and humidity carries out lateral blowing and evenly cools off the formation as-spun fibre.
With the as-spun fibre of processing in the spinning technique after over-richness is 10～15% high temperature resistant non-ignitibility finishes; Carry out multistage drafting through 2 counter extensioin rollers, drawing roller speed 2000～4000m/min, 20-250 ℃ of drawing roller temperature; Again through 140～160 ℃ of relaxation heat settings; Lax ratio is 1.0～1.1%, and over feed rate(OFR) is 0.7～1.4%, and winding speed is 4200～5000m/min.
The present invention compares with disclosed phase-change energy-storage fibre, and advantage is: attapulgite is bar-shaped loose structure, has superpower absorption property, and phase-change material and attapulgite are firmly combined, and phase-change material is difficult for oozing out; Do cooling curve research simultaneously with common polyamide fibre 6, find that the cooling velocity of phase-changing and temperature-regulating polyamide fibre 6 is starkly lower than common polyamide fibre 6, have good heat-storage thermoregulation function; Need not to add new equipment in this fiber production process in addition, technology is simple, and technology maturation is reliable.
The specific embodiment
In conjunction with accompanying drawing embodiment of the present invention is described further:
Embodiment 1: by phase-change material percentage by weight in the modified master batch is 10%; The attapulgite percentage by weight is 20%; Polycaprolactam weight resin percentage is 60%; Weight of additive percentage is 10% preparation modified master batch, and employing master batch syringe measures master batch and after becoming fibre with the blend of polycaprolactam resin slicer, sends into screw extruder and carry out fusion, and the blend ratio is 15: 85; After in course of conveying, fully mixing after the static mixing, carry out spinning, and carry out lateral blowing cooling, drawing-off and coiling.Wherein extruder temperature is 265 ℃, and spinning temperature is 270 ℃, and the lateral blowing temperature is 20 ± 2 ℃, and humidity is 80 ± 2%, and speed is 0.45m/s, and oil concentration is 10%, and drawing roller speed is 4000m/min, and 155 ℃ of heat setting temperatures are lax than 1.1.The spinning technique flow chart is seen accompanying drawing 2.The polyamide fibre of producing 6 specifications be 44dtex/36f, through detecting its physical index be: fracture strength 4.52cN/dtex, elongation at break 39.6%, boiling water shrinkage 8.8%, oil content is 0.9%; When this phase-changing and temperature-regulating polyamide fibre 6 arrived more than 100 ℃ in serviceability temperature, paraffin seepage phenomenon did not take place; Do cooling curve research simultaneously with common polyamide fibre 6, find that the cooling velocity of phase-changing and temperature-regulating polyamide fibre 6 is starkly lower than common polyamide fibre 6, so this modification polyamide fibre has tangible heat-accumulation temperature-adjustment effect.
Embodiment 2: by phase-change material percentage by weight in the modified master batch is 15%; The attapulgite percentage by weight is 20%; Polycaprolactam weight resin percentage is 50%; Weight of additive percentage is 15% preparation modified master batch, and employing master batch syringe measures master batch and after becoming fibre with the blend of polycaprolactam resin slicer, sends into screw extruder and carry out fusion, and the blend ratio is 20: 80; After in course of conveying, fully mixing after the static mixing, carry out spinning, and carry out lateral blowing cooling, drawing-off and coiling.Wherein extruder temperature is 255 ℃, and spinning temperature is 260 ℃, and the lateral blowing temperature is 20 ± 2 ℃, and humidity is 80 ± 2%, and speed is 0.45m/s, and oil concentration is 10%, and drawing roller speed is 3400m/min, and 150 ℃ of heat setting temperatures are lax than 1.05.The polyamide fibre of producing 6 specifications be 44dtex/36f, through detecting its physical index be: fracture strength 4.38cN/dtex, elongation at break 37.5%, boiling water shrinkage 8.4%, oil content is 0.8%; When this phase-changing and temperature-regulating polyamide fibre 6 arrived more than 100 ℃ in serviceability temperature, aliphatic acid seepage phenomenon did not take place; Do cooling curve research simultaneously with common polyamide fibre 6, find that the cooling velocity of phase-changing and temperature-regulating polyamide fibre 6 is starkly lower than common polyamide fibre 6, so this modification polyamide fibre has tangible heat-accumulation temperature-adjustment effect.
Claims (5)
1. the production method of an attapulgite modified phase-changing and temperature-regulating polyamide fibre 6 comprises the steps: to make modified master batch with becoming fibre with the polycaprolactam mixed with resin again through attapulgite absorption organic phase change material; Measure mixing with becoming fibre with the polycaprolactam resin slicer through the master batch syringe, make attapulgite modified phase-changing and temperature-regulating polyamide fibre 6 through operations such as melt spinning, drawing-off, cooling and shapings again.
2. attapulgite as claimed in claim 1 is characterized in that the attapulgite particle belongs to the inorganic particulate of the bar-shaped porous of nanoscale.
3. organic phase change material as claimed in claim 1 is a kind of in paraffin, aliphatic acid, the polyalcohol.
4. modified master batch as claimed in claim 1; It is characterized in that the organic phase change material percentage by weight is 1～10% in the master batch; The attapulgite percentage by weight is 30～60%, and polycaprolactam weight resin percentage is 20～60%, and weight of additive percentage is 1～10%.
5. attapulgite modified phase-changing and temperature-regulating polyamide fibre 6 as claimed in claim 1; The mass mixing ratio example that it is characterized in that modified master batch and polycaprolactam resin slicer is 15～25: 75～85, and in screw extruder, carrying out high temperature melt is the molten state spinning melt, and extruder temperature is 240～270 ℃; Fully mix in course of conveying through after the static mixing; Be injected into strand through filament spinning component again, spinning temperature is 240～270 ℃, and strand is 20 ± 5 ℃ through temperature; Humidity is 80 ± 5%, and wind speed is that the air-conditioning wind of 0.3～0.4 ℃ constant temperature and humidity carries out lateral blowing and evenly cools off the formation as-spun fibre; As-spun fibre is after over-richness is 10～15% high temperature resistant non-ignitibility finishes; Carry out multistage drafting through 2 counter extensioin rollers, drawing roller speed 2000～4000m/min, 20-250 ℃ of drawing roller temperature; Again through 140～160 ℃ of relaxation heat settings; Lax ratio is 1.0～1.1%, and over feed rate(OFR) is 0.7～1.4%, and winding speed is 4200～5000m/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106801266A (en) * | 2016-12-20 | 2017-06-06 | 武汉纺织大学 | Phase-change energy-storage fibre and preparation method thereof |
| CN108359411A (en) * | 2018-02-06 | 2018-08-03 | 中科院广州能源所盱眙凹土研发中心 | The preparation method of paraffin-attapulgite composite phase-change microcapsules |
| CN113186616A (en) * | 2021-07-01 | 2021-07-30 | 江苏恒力化纤股份有限公司 | Uvioresistant polyester industrial yarn and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102154737A (en) * | 2011-03-22 | 2011-08-17 | 天津工业大学 | Heat-accumulation temperature-regulation fiber and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102154737A (en) * | 2011-03-22 | 2011-08-17 | 天津工业大学 | Heat-accumulation temperature-regulation fiber and preparation method thereof |
Non-Patent Citations (3)
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| 《复合材料学报》 20091015 施韬等 "凹凸棒土吸附相变储能复合材料制备及其热物理性能表征" 第143-147页 1-5 第26卷, 第5期 * |
| 施韬等: ""凹凸棒土吸附相变储能复合材料制备及其热物理性能表征"", 《复合材料学报》 * |
| 邬国铭等: "《高分子材料加工工艺学》", 31 July 2000, 中国纺织出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106801266A (en) * | 2016-12-20 | 2017-06-06 | 武汉纺织大学 | Phase-change energy-storage fibre and preparation method thereof |
| CN108359411A (en) * | 2018-02-06 | 2018-08-03 | 中科院广州能源所盱眙凹土研发中心 | The preparation method of paraffin-attapulgite composite phase-change microcapsules |
| CN108359411B (en) * | 2018-02-06 | 2020-10-23 | 中科院广州能源所盱眙凹土研发中心 | Preparation method of paraffin-attapulgite composite phase change microcapsule |
| CN113186616A (en) * | 2021-07-01 | 2021-07-30 | 江苏恒力化纤股份有限公司 | Uvioresistant polyester industrial yarn and preparation method thereof |
| CN113186616B (en) * | 2021-07-01 | 2021-10-19 | 江苏恒力化纤股份有限公司 | Uvioresistant polyester industrial yarn and preparation method thereof |
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Application publication date: 20120801 |