CN106751783A - High visocity nylon 6 composite prepared by a kind of melting extrusion chain extending reaction and preparation method thereof - Google Patents
High visocity nylon 6 composite prepared by a kind of melting extrusion chain extending reaction and preparation method thereof Download PDFInfo
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- CN106751783A CN106751783A CN201611242189.0A CN201611242189A CN106751783A CN 106751783 A CN106751783 A CN 106751783A CN 201611242189 A CN201611242189 A CN 201611242189A CN 106751783 A CN106751783 A CN 106751783A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/05—Polymer mixtures characterised by other features containing polymer components which can react with one another
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/20—Recycled plastic
Abstract
High visocity nylon 6 composite prepared the invention discloses a kind of melting extrusion chain extending reaction and preparation method thereof, material prescription is made up of the component of following percentage by weight：PA6 97.5 100%；Tackifier 0 1.5%；Antioxidant 0 1%.Beneficial effects of the present invention are：1st, the PA6 of different viscosities is prepared by double screw extruder, simple to operate 2, the PA6 of different viscosities can be obtained by controlling the content of tackifier, the difference 3. for meeting demand of the different applications for PA6 viscosity reclaims nylon because it degrades during use, its viscosity is caused to decline, mechanical properties decrease, the viscosity and mechanical property for reclaiming nylon can be improved by melting extrusion chain extending reaction, increases its application.
Description
Technical field
The present invention relates to high visocity nylon 6 will be prepared using melting extrusion chain extending reaction, by controlling course of reaction in
The content of tackifier can obtain the nylon 6 of different viscosities, meet the different processing technology such as extrusion, injection, spinning for
The demand of the viscosity of nylon 6, and for the recovery raising of nylon 6, its viscosity increases its mechanical property, reuses it.
Background technology
Since polyamide realizes industrialization from the thirties in 20th century, in the side such as automobile, communication, electronic apparatus, mechanical industry
Face develops rapidly, and by the development of more than 70 years, yield was maximum during polyamide has turned into five large-engineering plastics, the most wide height of consumption
Molecular material.Nylon 6 as an important kind in polyamide product, due to its have oil resistant, chemical resistance, wearability,
The excellent performance such as good processability, is widely used in the parts such as gear, fan blade, high-pressure seal ring, oil pipe.
High visocity nylon has an excellent physical and mechanical properties, but the resin of nylon 6 that general polymerization is obtained
Molecular weight below 20,000, and engineering plastics are higher to the viscosity requirement of nylon resin, the shaping such as injection, extrusion, spinning
Technique is different to the viscosity requirement of nylon 6, and domestic production at present is generally fiber production, and resin producer is less, and greatly
Part low viscosity resin, so by increasing the grade of different viscosities nylon for meeting different productions for nylon viscosity
Demand has great importance.
The method for preparing high-viscosity nylon can be by changing polymerizing condition, at a higher temperature during extension reaction
Between, exclude small molecule in volatile materials, so as to improve molecular weight, this method reactant viscosity is larger, cause stirring and
Accessory substance diffusion is difficult, causes product quality to decline, improper from the economic viewpoint.Solid phase can also be used for improving nylon
Viscosity, even more than ten times of several times of the degree of polymerization, but this method reaction speed is slow, the time is long, and product quality is difficult to control.Expand
Chain agent refers to multiple functional groups with reactivity on same molecule, using chain extender and the different ends of nylon 6
Amido reaction, increase the viscosity of nylon 6, the method application is quick, effectively, in extruder several minutes complete extrusion chain extension it is anti-
Should, it is simple and easy to apply, it is adapted to large-scale industrial production.
The content of the invention
High visocity nylon 6 prepared the invention provides a kind of melting extrusion chain extending reaction and preparation method thereof, using one
Planting ethene and activity numerous in the copolymer of maleic anhydride can realize increasing dividing for PA6 with the amido reaction of the end of nylon 6
Son amount, so as to improve its viscosity, realizes that nylon 6 is viscous to nylon 6 in different moulding process such as injection, extrusion, spinning and blowings
The demand of degree, and applied in nylon 6 is reclaimed, its mechanical property is improved by increasing viscosity, reclaimed materials can be improved
Secondary utilization.
The present invention is the proposed technical problem of solution, the technical scheme for using for：
High visocity nylon 6 composite prepared by a kind of melting extrusion chain extending reaction, it include it is following by weight percentage
The raw material of meter：
PA6 97.5-100%；
Tackifier 0-1.5%
Antioxidant 0-1%.
The PA6 both can be that synthesis without the PA6 for using can also reclaim nylon 6, reclaim nylon 6 by following
Mode is obtained：
First the component containing PA6 is sorted out from the carpet being collected into, is then crushed by dry type cutter,
Latex and calcium carbonate are separated from carpet is reclaimed, (the patent No. is processed finally by the wet separation technology of patent：
The Bl of US 7,784,719), then extruding pelletization is recycled the raw material of waste carpet nylon 6.
The density for reclaiming waste carpet nylon 6 therein is 1.17g/cm^3, residues of combustion≤6%, and tensile strength is
58MPa, (method of testing ISO527-2), notch impact strength is 3.0KJ/m^2 (method of testing ISO 179), bending strength
85MPa, bending modulus 2200MPa (method of testing ISO 178, speed 2mm/min).
Described tackifier are a kind of ethene and maleic anhydride 1:1 alternate copolymer, there is more than 200 on a strand
Active reaction functional group.For the dispersion in increasing tackifier during the course of the reaction, tackifier are made into active ingredient in advance and is contained
The master batch of amount 25%, carrier is nylon 6.
The functional aids such as lubricant, antioxidant are may also include in described material.
The preparation method of high visocity nylon 6 composite prepared by above-mentioned melting extrusion chain extending reaction, comprises the following steps：
(1) dried each raw material is weighed by formula rate to be well mixed by homogenizer；
(2) the above-mentioned raw material for mixing is added by the main spout of double screw extruder, by melting extrusion, is made
Described high visocity nylon 6 is obtained after the operations such as grain, dried process.
Compared with prior art, advantage of the invention is that：High visocity nylon it is general by changing polymeric reaction condition
Or obtained by solid-phase polymerization, both mode consersion units are complicated, and product quality is difficult to control, by melting extrusion
Chain extending reaction prepares high visocity nylon has equipment simple, reclaims nylon and is degraded during use due to it, causes it to glue
Degree declines, mechanical properties decrease, and the viscosity and mechanical property for reclaiming nylon can be improved by melting extrusion chain extending reaction, increases
Its application.
Specific embodiment
In order that the technical problem to be solved in the present invention, technical scheme and beneficial effect are clearer, below in conjunction with reality
Example is applied, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used for explaining this hair
It is bright, it is not intended to limit the present invention.
Embodiments of the invention use following materials：
Waste carpet reclaims PA6, WELLMAN Plastics Recycling, LLC；
PA6 MF800 Jiangsu Rui Meifu Industrial Co., Ltd.s；
Antioxidant：Hinered phenols antioxidant 1010, CIBA companies of Switzerland；
Antioxidant：Three [2.4- di-tert-butyl-phenyls] phosphite esters 168, it is commercially available.
Properties of product method of testing：
Melt mass flow index (melt index)：By ISO1133-1 methods, tested under 230 DEG C, 5kg load.
Inherent viscosityWherein η r are relative viscosity, and η sp are specific viscosity η sp=η r-1, c
It is solution concentration
Tensile property：By ISO527-2 methods, batten size：170*10*4mm, test speed 5mm/min.
Bending property：By ISO178-1 methods, batten size：80*10*4mm, test speed 2mm/min.
Notched impact properties：By the methods of ISO 180, batten size：80*10*4mm.
Embodiment 1：
PA6 MF800 4.925kg are weighed in drying 4h at 100 DEG C, tackifier 25g, antioxidant 1010 and 168 each
12.5g, lubricant 25g are well mixed in homogenizer, obtain resin compound.
By main spout above-mentioned well mixed resin compound is added into double screw extruder, and (screw diameter is
35mm, draw ratio is L/D=36) in, each section of control temperature (being exported to head from charge door) of double screw extruder is 190
DEG C, 200 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, double screw extruder turn
Speed is 360r/min, and pelletizing obtains product after the material strip of extrusion is through water-carrying groove cooling, forced air drying agent is dried.
Standard batten is molded at a temperature of 235 DEG C after above-mentioned material is dried into 4h in 110 DEG C in air dry oven.
By the mechanical property batten of injection formed in laboratory standard environment (23 DEG C, 50%RH), it is laggard that placement 24h carries out status adjustment
Row test.Above-mentioned dried material is tested into melting means under conditions of 230 DEG C/5kg, and material is tested using Ubbelohde viscometer
The relative viscosity of material, the intrinsic viscosity of material is calculated using formula, above test result is shown in Table 1.
Embodiment 2：
PA6 MF800 4.9kg are weighed in drying 4h at 100 DEG C, tackifier 50g, antioxidant 1010 and 168 each 12.5g,
Lubricant 25g is well mixed in homogenizer, obtains resin compound.
By main spout above-mentioned well mixed resin compound is added into double screw extruder, and (screw diameter is
35mm, draw ratio is L/D=36) in, each section of control temperature (being exported to head from charge door) of double screw extruder is 190
DEG C, 200 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, double screw extruder turn
Speed is 360r/min, and pelletizing obtains product after the material strip of extrusion is through water-carrying groove cooling, forced air drying agent is dried.
Standard batten is molded at a temperature of 235 DEG C after above-mentioned material is dried into 4h in 110 DEG C in air dry oven.
By the mechanical property batten of injection formed in laboratory standard environment (23 DEG C, 50%RH), it is laggard that placement 24h carries out status adjustment
Row test.Above-mentioned dried material is tested into melting means under conditions of 230 DEG C/5kg, and material is tested using Ubbelohde viscometer
The relative viscosity of material, the intrinsic viscosity of material is calculated using formula, above test result is shown in Table 1.
Embodiment 3：
PA6 MF800 4.875kg are weighed in drying 4h at 100 DEG C, tackifier 75g, antioxidant 1010 and 168 each
12.5g, lubricant 25g are well mixed in homogenizer, obtain resin compound.
By main spout above-mentioned well mixed resin compound is added into double screw extruder, and (screw diameter is
35mm, draw ratio is L/D=36) in, each section of control temperature (being exported to head from charge door) of double screw extruder is 190
DEG C, 200 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, double screw extruder turn
Speed is 360r/min, and pelletizing obtains product after the material strip of extrusion is through water-carrying groove cooling, forced air drying agent is dried.
Standard batten is molded at a temperature of 235 DEG C after above-mentioned material is dried into 4h in 110 DEG C in air dry oven.
By the mechanical property batten of injection formed in laboratory standard environment (23 DEG C, 50%RH), it is laggard that placement 24h carries out status adjustment
Row test.Above-mentioned dried material is tested into melting means under conditions of 230 DEG C/5kg, and material is tested using Ubbelohde viscometer
The relative viscosity of material, the intrinsic viscosity of material is calculated using formula, above test result is shown in Table 1.
Embodiment 4：
Weigh waste carpet and reclaim PA6 4.9kg in drying 4h at 100 DEG C, tackifier 50g, antioxidant 1010 and 168 each
12.5g, lubricant 25g are well mixed in homogenizer, obtain resin compound.
By main spout above-mentioned well mixed resin compound is added into double screw extruder, and (screw diameter is
35mm, draw ratio is L/D=36) in, each section of control temperature (being exported to head from charge door) of double screw extruder is 190
DEG C, 200 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, double screw extruder turn
Speed is 360r/min, and pelletizing obtains product after the material strip of extrusion is through water-carrying groove cooling, forced air drying agent is dried.
Standard batten is molded at a temperature of 235 DEG C after above-mentioned material is dried into 4h in 110 DEG C in air dry oven.
By the mechanical property batten of injection formed in laboratory standard environment (23 DEG C, 50%RH), it is laggard that placement 24h carries out status adjustment
Row test.Above-mentioned dried material is tested into melting means under conditions of 230 DEG C/5kg, and material is tested using Ubbelohde viscometer
The relative viscosity of material, the intrinsic viscosity of material is calculated using formula, above test result is shown in Table 1.
Comparative example 1：
PA6 MF800 4.95kg are weighed in drying 4h, antioxidant 1010 and 168 each 12.5g, lubricant 25g at 100 DEG C
It is well mixed in homogenizer, obtains resin compound.
By main spout above-mentioned well mixed resin compound is added into double screw extruder, and (screw diameter is
35mm, draw ratio is L/D=36) in, each section of control temperature (being exported to head from charge door) of double screw extruder is 190
DEG C, 200 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, double screw extruder turn
Speed is 360r/min, and pelletizing obtains product after the material strip of extrusion is through water-carrying groove cooling, forced air drying agent is dried.
Standard batten is molded at a temperature of 235 DEG C after above-mentioned material is dried into 4h in 110 DEG C in air dry oven.
By the mechanical property batten of injection formed in laboratory standard environment (23 DEG C, 50%RH), it is laggard that placement 24h carries out status adjustment
Row test.Above-mentioned dried material is tested into melting means under conditions of 230 DEG C/5kg, and material is tested using Ubbelohde viscometer
The relative viscosity of material, the intrinsic viscosity of material is calculated using formula, above test result is shown in Table 1.
Comparative example:2：
Weigh waste carpet and reclaim PA6 4.95kg in 4h, antioxidant 1010 and 168 each 12.5g are dried at 100 DEG C, lubricate
Agent 25g is well mixed in homogenizer, obtains resin compound.
By main spout above-mentioned well mixed resin compound is added into double screw extruder, and (screw diameter is
35mm, draw ratio is L/D=36) in, each section of control temperature (being exported to head from charge door) of double screw extruder is 190
DEG C, 200 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, double screw extruder turn
Speed is 360r/min, and pelletizing obtains product after the material strip of extrusion is through water-carrying groove cooling, forced air drying agent is dried.
Standard batten is molded at a temperature of 235 DEG C after above-mentioned material is dried into 4h in 110 DEG C in air dry oven.
By the mechanical property batten of injection formed in laboratory standard environment (23 DEG C, 50%RH), it is laggard that placement 24h carries out status adjustment
Row test.Above-mentioned dried material is tested into melting means under conditions of 230 DEG C/5kg, and material is tested using Ubbelohde viscometer
The relative viscosity of material, the intrinsic viscosity of material is calculated using formula, above test result is shown in Table 1.
Table 1：The performance test results.
Be can be seen that from data shown in table can by the contrast of embodiment 1, embodiment 2, embodiment 3 and comparative example 1
Go out, the consumption with tackifier increases, inherent viscosity increases, melting means reduction, this is just illustrated can be by controlling the use of tackifier
Amount prepares the nylon 6 of different viscosities by melting extrusion chain extending reaction, and viscosity increase, mechanical property also can slightly increase
Plus.By comparative example 1 and comparative example 2 it can be found that reclaim nylon 6 mechanical property it is low, viscosity is low, and melting means is high, this be due to
Reclaim nylon 6 and occur what degraded was caused during processing and use.Be can be seen that by comparative example 4 and comparative example 2
While tackifier improve its viscosity for reclaiming nylon, its mechanical property can be also increased substantially, increase and reclaim answering for nylon
With value.It can thus be seen that high visocity nylon 6 equipment is prepared simply by melting extrusion chain extending reaction, it is operable using wide
Property it is strong, with very strong industrial application value.
Claims (8)
1. the high visocity nylon 6 composite that prepared by a kind of melting extrusion chain extending reaction, it is characterised in that：It includes following by weight
Measure the raw material of percentages：
PA6 97.5-100%；
Tackifier 0-1.5%
Antioxidant 0-1%.
2. the high visocity nylon 6 composite that prepared by a kind of melting extrusion chain extending reaction according to claim 1, its feature
It is：The PA6 both can be synthesis without the PA6 for using can also be reclaim nylon 6.
3. the high visocity nylon 6 composite that prepared by a kind of melting extrusion chain extending reaction according to claim 2, its feature
It is：The recovery nylon 6 is obtained in the following manner：
First the component containing PA6 is sorted out from the carpet being collected into, then crushed by dry type cutter, by breast
Glue and calcium carbonate are separated from carpet is reclaimed, and are processed finally by the wet separation technology of patent, and then extrusion is made
Grain is recycled the raw material of waste carpet nylon 6.
4. the high visocity nylon 6 composite that prepared by a kind of melting extrusion chain extending reaction according to claim 2, its feature
It is：The described density for reclaiming waste carpet nylon 6 is 1.17g/cm^3, and residues of combustion≤6%, tensile strength is 58M
Pa, notch impact strength is 3.0KJ/m^2, bending strength 85MPa, bending modulus 2200M Pa.
5. the high visocity nylon 6 composite that prepared by a kind of melting extrusion chain extending reaction according to claim 1, its feature
It is：Described tackifier are a kind of ethene and maleic anhydride 1:1 alternate copolymer, has more than 200 to live on a strand
Property reactive functionality.
6. the high visocity nylon 6 composite that prepared by a kind of melting extrusion chain extending reaction according to claim 5, its feature
It is：Tackifier are first made the master batch of active constituent content 25%, carrier is nylon 6.
7. the high visocity nylon 6 composite that prepared by a kind of melting extrusion chain extending reaction according to claim 1, its feature
It is：Lubricant, antioxidant functional aid are may also include in described material.
8. the high visocity nylon 6 composite that prepared by one of any described melting extrusion chain extending reactions of claim 1-7, it is special
Levy and be：Comprise the following steps：
(1) dried each raw material is weighed by formula rate to be well mixed by homogenizer；
(2) the above-mentioned raw material for mixing is added by the main spout of double screw extruder, by melting extrusion, granulation, is done
Described high visocity nylon 6 is obtained after the operations such as dry treatment.
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| CN201611242189.0A CN106751783A (en) | 2016-12-29 | 2016-12-29 | High visocity nylon 6 composite prepared by a kind of melting extrusion chain extending reaction and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108047707A (en) * | 2017-12-28 | 2018-05-18 | 南京聚隆科技股份有限公司 | A kind of high-strength wearable injection-level nylon and preparation method |
| CN110483984A (en) * | 2019-08-22 | 2019-11-22 | 杭州异彩新材料有限公司 | A kind of modified enhancing Wear-resistant corrosion-resistant polycaprolactam material, preparation method and application |
| CN111205636A (en) * | 2020-02-28 | 2020-05-29 | 金旸（厦门）新材料科技有限公司 | Polyamide material and preparation method and application thereof |
| CN114539519A (en) * | 2022-03-28 | 2022-05-27 | 华润化学材料科技股份有限公司 | High-barrier nylon and preparation method and application thereof |
| CN114752213A (en) * | 2022-05-23 | 2022-07-15 | 江苏瑞美福新材料有限公司 | Environment-friendly economic copolymerized nylon modified material |
| CN114836027A (en) * | 2022-04-25 | 2022-08-02 | 宁波坚锋新材料有限公司 | High-viscosity recycled nylon recovered from fishing net wires and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108047707A (en) * | 2017-12-28 | 2018-05-18 | 南京聚隆科技股份有限公司 | A kind of high-strength wearable injection-level nylon and preparation method |
| CN110483984A (en) * | 2019-08-22 | 2019-11-22 | 杭州异彩新材料有限公司 | A kind of modified enhancing Wear-resistant corrosion-resistant polycaprolactam material, preparation method and application |
| CN111205636A (en) * | 2020-02-28 | 2020-05-29 | 金旸（厦门）新材料科技有限公司 | Polyamide material and preparation method and application thereof |
| CN111205636B (en) * | 2020-02-28 | 2021-11-19 | 金旸（厦门）新材料科技有限公司 | Polyamide material and preparation method and application thereof |
| CN114539519A (en) * | 2022-03-28 | 2022-05-27 | 华润化学材料科技股份有限公司 | High-barrier nylon and preparation method and application thereof |
| CN114539519B (en) * | 2022-03-28 | 2023-09-26 | 华润化学材料科技股份有限公司 | High-barrier nylon and preparation method and application thereof |
| CN114836027A (en) * | 2022-04-25 | 2022-08-02 | 宁波坚锋新材料有限公司 | High-viscosity recycled nylon recovered from fishing net wires and preparation method thereof |
| CN114752213A (en) * | 2022-05-23 | 2022-07-15 | 江苏瑞美福新材料有限公司 | Environment-friendly economic copolymerized nylon modified material |
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