CN102161755A - Nylon-6 resin, nylon-6 fiber and preparation method thereof - Google Patents
Nylon-6 resin, nylon-6 fiber and preparation method thereof Download PDFInfo
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- CN102161755A CN102161755A CN 201110073191 CN201110073191A CN102161755A CN 102161755 A CN102161755 A CN 102161755A CN 201110073191 CN201110073191 CN 201110073191 CN 201110073191 A CN201110073191 A CN 201110073191A CN 102161755 A CN102161755 A CN 102161755A
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- 229920002292 Nylon 6 Polymers 0.000 title claims abstract description 112
- 239000000835 fiber Substances 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920005989 resin Polymers 0.000 title abstract description 17
- 239000011347 resin Substances 0.000 title abstract description 17
- 238000009987 spinning Methods 0.000 claims abstract description 62
- 239000000463 material Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 37
- 229910052751 metal Inorganic materials 0.000 claims abstract description 27
- 239000002184 metal Substances 0.000 claims abstract description 27
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 26
- 238000002074 melt spinning Methods 0.000 claims abstract description 25
- 150000001875 compounds Chemical class 0.000 claims abstract description 23
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical group O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims abstract description 20
- -1 phosphate radical Chemical class 0.000 claims description 61
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 43
- 238000001035 drying Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- 238000007142 ring opening reaction Methods 0.000 claims description 14
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 8
- 229910019142 PO4 Inorganic materials 0.000 claims description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 8
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- 239000013110 organic ligand Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 239000010452 phosphate Substances 0.000 claims description 8
- 229910052717 sulfur Chemical group 0.000 claims description 8
- 239000011593 sulfur Chemical group 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 7
- 239000003381 stabilizer Substances 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 5
- 239000011575 calcium Substances 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 2
- 238000009941 weaving Methods 0.000 abstract description 5
- 150000002739 metals Chemical class 0.000 abstract 2
- 229920001778 nylon Polymers 0.000 description 36
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- 238000001125 extrusion Methods 0.000 description 13
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- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 7
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- 238000004519 manufacturing process Methods 0.000 description 7
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- 238000003860 storage Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
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- 238000001291 vacuum drying Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000012752 auxiliary agent Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000004594 Masterbatch (MB) Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
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- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- UBXAKNTVXQMEAG-UHFFFAOYSA-L strontium sulfate Chemical compound [Sr+2].[O-]S([O-])(=O)=O UBXAKNTVXQMEAG-UHFFFAOYSA-L 0.000 description 2
- 229920002972 Acrylic fiber Polymers 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 229920004935 Trevira® Polymers 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 description 1
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 1
- 239000001639 calcium acetate Substances 0.000 description 1
- 229960005147 calcium acetate Drugs 0.000 description 1
- 235000011092 calcium acetate Nutrition 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 150000007520 diprotic acids Chemical class 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000004811 fluoropolymer Substances 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- 239000011654 magnesium acetate Substances 0.000 description 1
- 235000011285 magnesium acetate Nutrition 0.000 description 1
- 229940069446 magnesium acetate Drugs 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- 229960001708 magnesium carbonate Drugs 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 229910000400 magnesium phosphate tribasic Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
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- 239000000178 monomer Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
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- 238000007781 pre-processing Methods 0.000 description 1
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- 238000005728 strengthening Methods 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 229910001631 strontium chloride Inorganic materials 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 description 1
- 229910001866 strontium hydroxide Inorganic materials 0.000 description 1
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- JOPDZQBPOWAEHC-UHFFFAOYSA-H tristrontium;diphosphate Chemical compound [Sr+2].[Sr+2].[Sr+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JOPDZQBPOWAEHC-UHFFFAOYSA-H 0.000 description 1
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Abstract
The invention relates to the field of spinning materials, and firstly provides a nylon-6 resin which is prepared by the polymerization reaction of a caprolactam monomer and fixed melt of compounds of metals in the second main group, wherein based on the total weight of the caprolactam monomer, the weight of the compounds of metals in the second main group is 0.01-1.0%. The invention also provides a nylon-6 fiber which is prepared from the nylon-6 resin by melt spinning. By using the nylon-6 resin and the preparation method provided by the invention, the fine-denier or superfine-denier nylon-6 fiber with a fineness of about 0.10-1.0dtex can be obtained. Both the strength and the breaking elongation of the fiber conform to post-weaving requirements. Besides, the invention fills up the gap that the fine-denier/superfine-denier nylon-6 filament can not be produced by the conventional high-speed spinning method home and abroad, and increases the technological content and added value of the nylon-6 fiber product.
Description
Technical field
The present invention relates to the spinning material field, relate in particular to and be specifically designed to a kind of Nylon 6 of producing thin dawn or super fine denier nylon 6 fiber, nylon 6 fiber and preparation method thereof.
Background technology
In general, can the weave macromolecular material of usefulness comprises nylon (polymeric amide), polypropylene, polyethylene terephthalate and polyacrylonitrile etc.These materials can form fiber and nylon, polypropylene fibre, terylene and acrylic fibers etc. by spinning processing, thereby are used for textile industry.Melt-spinning is a kind of spinning processes commonly used, by melt-spinning can obtain being suitable for weaving each fibrid of usefulness.Usually, use the filament number of the fiber that melt spinning method obtains to reach 1.0dtex.With the fibrous woven of such fiber number product, for example garment material etc. have lot of advantages, so the application space, market is wide.
Yet, also more and more higher along with the raising of people's living standard for the requirement of textiles, be starved of some existing defectives that can overcome textiles.For example, above-mentioned mention such as products such as garment materials, because therefore its fiber yarn slightly exists that feel is coarse, flexibility is poor, ventilation property is poor, water-absorbent is poor, is easy to problem such as pilling.In order to address these problems, it is an important subject that the thin dawn of textile fibres or super fine denier change into.
At present, carried out a lot of researchs, and a lot of relevant reports have been arranged about thin dawn of textile fibres or super fine denierization.For example, on the Chinese side, thin dawn of trevira or super fine denier technology in century the eighties succeed in developing.The thin dawn of polypropylene fibre or super fine denierization in last century the nineties develop by the Chinese Academy of Sciences chemistry Xu Duan husband academician of institute, this technology has realized industrialization at present, and correlation technique information is to describe to some extent in the Chinese patent literature of CN1073595A, CN1058062A, CN1076032A and CN1068075A at publication number.
But for nylon fiber, the technology of utilization fusion direct fabrics method manufacturing (surpassing) fine denier nylon fiber is still immature.
Characteristics such as the nylon fiber fabric has absorbing sweat, lightweight, toughness is good, rebound resilience good, antiacid alkali are best suited for one of man-made fabric of human dress.Application on clothes also is one of main application of nylon fiber.The thickness of nylon fiber can be characterized with filament number, usually, filament number be man-made fiber about 1.1dtex fine count fiber, and filament number to be man-made fiber about 0.55dtex be called superfine Denier fibre.Nylon fiber is thin more, and the snugness of fit of its fabric is good more.Thin dawn or superfine denier nylon fibre can be made into soft, comfortable and easy to wear high-grade yarn fabric, and very high economic worth is arranged.Thereby the exploitation of fine count fiber and superfine Denier fibre manufacturing technology is the new and high technology all paid attention to of each state in recent years.If can realize fusion direct fabrics method thin dawn of manufacturing or superfine denier nylon fibre, that will open up another wide Application Areas for textile industry.
The diameter of fine count fiber and superfine Denier fibre is much thinner than conventional chemical fiber (filament number is generally 3-6 about the dawn), and the technical difficulty of making this class man-made fiber is quite big, need select appropriate spinning material and auxiliary agent for use.Also need the technical scheme and the strict control spinning of choose reasonable spinning, every production process such as drawing-off.
Yet up to the present, the research report that improves the nylon spinning property by modification mode is also few, thereby the main aspect of modification is by copolymerization or adds auxiliary agent and reduce the extension ability that the molecular orientation of nylon when reeling improves monofilament.For example, (1) introduces asymmetric cell by copolymerization, reducing the ability of molecular orientation, as, add the caprolactam and the assorted hexane of azo-cycle of asymmetric diprotic acid, diamine or band side group during common nylon polymerization; (2) when spinning, add acrylic acid derivative, as the methyl methacrylate polyester; (3) the employing long-chain nylon carries out spinning or add long-chain nylon and salt thereof or the like when the monomer polymerization of matrix nylon.
On the other hand, the improvement in spinning process mainly contain following aspect: (1) reduces the aperture of spinning jet, as using the diameter 0.2mm even the spinning jet of fine pore more, and the hole count of corresponding increase spinning jet; (2) filter to improve the purity of spinning melt by high precision; (3) reduce spray silk level of stretch and degree of molecular orientation of tow in the winding process and extend abilities with more reservation tow; (4) take higher drafting multiple.
The nylon fiber fabric is best suited for one of man-made fabric of human dress.Therefore, the nylon fiber monofilament is carried out the thin dawn or super fine denierization extremely important.And it is very important beyond doubt for producing thin dawn or superfine denier nylon fibre to propose suitable spinning material.
, with regard to mentioned prior art, all can't be reasonably with thin dawn of nylon fiber or super fine denierization, the fiber number of gained fiber is generally still at least greater than 1.0dtex.
In addition, the contriver develops a kind of master batch auxiliary agent before this, this master batch auxiliary agent is to be formed by metallic compound and nylon matrix thorough mixing melt-processed, utilizes this master batch auxiliary agent and nylon particle to carry out direct scorification spinning, can reach the purpose of spinning denier/superfine denier nylon long filament.Correlation technique has been applied for patent, and detailed technology information is to elaborate in the patent documentations such as CN101122053A, CN101139750A, CN101311389A, CN101724265A at publication number.
Summary of the invention
Deficiency at above-mentioned prior art existence, the object of the present invention is to provide a kind of Nylon 6 that is used for producing thin dawn or super fine denier nylon 6 fiber, and carry out melt-spinning by this resin and produce thin dawn or the super fine denier nylon 6 fiber of fiber number less than 1.0dtex.
Another object of the present invention is to provide a kind of preparation method who produces thin dawn or super fine denier nylon 6 fiber.
The objective of the invention is to be implemented by the following technical programs:
A kind of Nylon 6 is that the blend melt by the compound of the caprolactam monomer and second main group metal makes through polyreaction, and wherein, based on caprolactam monomer gross weight meter, the weight of the compound of second main group metal is 0.01～1.0%.
Major technique design of the present invention is, by in caprolactam monomer, adding a kind of compound of second main group metal, the compound of an amount of second main group metal directly is dissolved in the hexanolactam melt, obtain to produce the resin dedicated of thin dawn or super fine denier nylon 6 fiber by the ring opening agent initiated polymerization again after being uniformly dispersed, described resin dedicated main component is the nylon-6 matrix body that is polymerized by caprolactam monomer, this is resin dedicated to have extraordinary performance, for example can directly be spun into thin dawn or superfine denier nylon fibre by method of the present invention.
Discover, the affiliation that adds of the compound of second main group metal makes nylon 6 melts show good performance in the melt-spinning process, for example high strength, high viscosity, high tensile deformation and high spinning property etc., thus make Nylon 6 of the present invention can be spun into thin dawn or the super fine denier nylon 6 fiber of fiber number less than 1.0dtex.Can be spun into the effect of thin dawn or superfine denier nylon fibre in order to ensure Nylon 6, the usage quantity of the compound of second main group metal is as follows: based on used caprolactam monomer gross weight meter, the compound weight of second main group metal is 0.01～1.0wt%, be preferably 0.1%～0.6wt%, more preferably 0.2%～0.4wt%.If the usage quantity of the compound of second main group metal is lower than 0.01wt%, then its modified effect to nylon is good inadequately, causes the special-purpose nylon resin to be difficult to be spun into thin dawn or superfine denier nylon fibre; If the usage quantity of the compound of second main group metal is greater than 1.0wt%, then the amount of the compound of second main group metal of Tian Jiaing is too much, makes that resin dedicated molecular weight distribution is irregular, and the spinning effect variation causes filametntary degradation.
As preferably, according to a kind of Nylon 6 of the present invention, wherein, the compound of described second main group metal is second main group metal salt or the complex compound, wherein, described second main group metal is selected from magnesium, calcium or strontium, the negatively charged ion of the described second main group metal salt or the part of complex compound are selected from hydroxide radical, phosphate radical, carbonate, carboxylate radical, nitrate radical, sulfate radical, acetate moiety, sulfonate radical, inferior sulfate radical, halide anion, pseudohalogen ion (for example, thiocyanate ion) and other are nitrogenous and/or contain oxygen (as carboxylate radical) and/or sulfur-bearing organic ligand or polynary part.Particularly, the examples for compounds indefiniteness of described second main group metal comprises: magnesium hydroxide, calcium hydroxide, strontium hydroxide; Magnesiumcarbonate, lime carbonate, Strontium carbonate powder; Trimagnesium phosphate, calcium phosphate, strontium phosphate; Magnesium acetate, calcium acetate, strontium acetate; Sal epsom, calcium sulfate, Strontium Sulphate; Sulfonic acid magnesium, calcium sulphonate, sulfonic acid strontium; Magnesium chloride, calcium chloride, strontium chloride etc.
As preferably, according to a kind of Nylon 6 of the present invention, wherein, add ring opening agent and molecular weight stabilizer in the described polyreaction, wherein, described ring opening agent is meant distilled water or deionized water, the addition of ring opening agent accounts for 1～5% of caprolactam monomer gross weight, is preferably 2～4%; Described molecular weight stabilizer is meant acetic acid or/and hexanodioic acid, and the addition of molecular weight stabilizer accounts for 0.1～0.5% of caprolactam monomer gross weight, is preferably 0.2～0.4%.The polymerization of Nylon 6 of the present invention mainly causes the caprolactam monomer polymerization by ring opening agent, is aided with the regulation and control that molecular weight stabilizer carries out the fluoropolymer resin molecular weight.
As preferably, according to a kind of Nylon 6 of the present invention, wherein, in the described polyreaction: temperature control divides three phases, material is at the straight type successive polymerization of normal pressure pipe (being called for short straight type VK pipe) epimere, and temperature is controlled between 230～300 ℃, is preferably 230～290 ℃, be beneficial to heat up caprolactam monomer open loop and draining; In straight type VK pipe stage casing, temperature is controlled between 240～290 ℃, is preferably 240～280 ℃, is beneficial to the growth of molecular chain; At straight type VK pipe hypomere, temperature is controlled between 220～270 ℃, is preferably 230～265 ℃, is beneficial to the raising of resin molecular-weight average and the content of low-molecular material.By temperature and the polymerization time (being generally 10-20hr) of controlling straight type VK pipe, obtain the purpose of the resin of suitable molecular weight and molecular weight distribution with realization.
It is a kind of by the nylon 6 fiber of above-mentioned Nylon 6 through the melt spinning method preparation that the present invention also provides.Nylon 6 of the present invention adopts direct melt spinning method, can produce thin dawn or super fine denier nylon 6 fiber on common high-speed spinning equipment, and the intensity of fiber and elongation at break all meet the back requirements of weaving process.
As preferably, according to nylon 6 fiber of the present invention, wherein, the fiber number of described nylon 6 fiber is 0.1～1.0dtex.Optimize the performance quality of nylon 6, can enlarge its range of application.
The present invention also provides a kind of preparation method of above-mentioned nylon 6 fiber, comprise: Nylon 6 is carried out melt-spinning, wherein, in the melt-spinning process: the temperature of nylon 6 molten masses is between 130～320 ℃, more preferably in 180～280 ℃ of scopes, most preferably in 250～270 ℃ of scopes; The hole count of spinning jet is 10～150, and the aperture is 0.1～0.6mm, and the spinning jet length-to-diameter ratio is 2.0～4.0; The speed of reeling is 2000～6000m/min.The reason of each parameter is with reference to conventional nylon spinning parameter in the control melt spinning method, in conjunction with the performance of denier/superfine denier nylon fiber, and corresponding changing.For example, single fiber is thin, need reduce orifice diameter, thereby reduces the spinneret draft multiple, and tow is not ruptured; The resin that contains metal-salt, the corresponding increase of melt viscosity for improving fluidity of molten, needs correspondingly heighten spinning temperature 5-10 ℃ etc.
As preferably, according to the preparation method of nylon 6 fiber of the present invention, wherein, before the described melt-spinning Nylon 6 is carried out drying, to remove moisture and small-molecule substance, drying temperature is 90-100 ℃, be 24-48 hour time of drying.
Preparation method of the present invention, operation is simple, be convenient to operation, can obtain thin dawn or the super fine denier nylon 6 fiber of fiber number less than 1.0dtex, and in preparation process, the nylon 6 fiber tow can not rupture basically, and the mechanical property of thin dawn of gained or super fine denier nylon 6 fiber is fine, and fiber number is minimum can to reach about 0.1dtex.
As preferably, according to the preparation method of nylon 6 fiber of the present invention, wherein, also do hot drawing-off before the described coiling, the temperature of hot drawing-off is between 50-170 ℃.Controlling hot drawing temperature is to make temperature be higher than the second-order transition temperature of nylon fiber in the reason of this scope, so that fiber segment sufficient movement, orientation degree, the degree of order increase; But when temperature was too high, fiber was easy to fusing, and strength degradation makes the tow fracture.The advantage that increases hot this operation of drawing-off is to increase fiber segment motor capacity, and the fibre orientation degree is increased, and degree of crystallinity improves, thereby the intensity of fortifying fibre in addition, also can suitably reduce the fiber number of fiber, obtains the littler fiber of filament number.
Term " fiber number " is used for representing the thickness degree of nylon fiber herein, represents with " dtex " usually." dtex " is the unit of fiber number, and 1dtex is meant that the fiber quality of long 10000m is 1 gram.
Term " melt spinning method " is meant the raw material heating and melting that spinning is used herein, molten mass is delivered to spinning-drawing machine after extruding by screw extrusion press, quantitatively be pressed into molten mass in the spinning components through volume pump, by the orifice on the spinning jet nylon 6 melts are extruded with the filament attitude, the cross air blow cooling forming, obtain finished product through oil boundling and coiling again, also through overheated drawing-off, promptly get thin dawn or super fine denier nylon 6 fiber behind the boundling that perhaps oils.
Term " melt-spinning process " comprises from former and expects all processes that become silk herein, for example the melting process that will carry out preprocessing process that raw material that spinning uses carries out, raw material and molten mass is become the silk process.
The word of the expression scope of Chu Xianing herein, as " less than ", " greater than " and " ... in the scope " etc., its represented scope comprises the endpoint value of respective range.
The compound that adds second main group metal can obviously improve the spinning property and the weaving security of nylon 6, thereby can obtain thin dawn or the super fine denier nylon 6 fiber of fiber number less than 1.0dtex.The contriver thinks that possible mechanism is as follows: the compound of second main group metal can with nylon 6 molecule generation complex coordination effects, change the melt structure of nylon, improve the intensity of nylon 6 melts, improve the viscosity of molten mass, reduce melt flow index MFI, thereby make it can bear bigger drawing force, even when nylon 6 melts become the fritting body behind the spray silk, still have tensile strength preferably, therefore can tolerate bigger drawing force, the tension force that makes fibre bundle in the melt-spinning process, can bear in the drawing step to be born and can not rupturing, thereby improve the spinning property of nylon, obtain thin dawn or super fine denier nylon 6 fiber.But effect of the present invention is not subjected to the constraint of this theory.
The present invention compared with prior art has the following advantages:
1. the present invention adopts and add properties-correcting agent metallic salt material before the caprolactam monomer polymerization, thereby makes special-purpose nylon 6 resins after polymerization is finished.Metallic salt can change nylon 6 melt structures, the tensile strength of while Reinforced Nylon 6 melts, and the crystallization rate of reduction nylon 6 melts can be produced denier/superfine denier nylon 6 long filaments thereby provide a kind of on common high-speed spinning equipment; The resulting ultra-fine fibre of the present invention can be contained plurality of specifications, has stable excellent properties, weaves the different demands of arrangement processing after can satisfying, the ultra-fine fibre kind of the present invention's exploitation, also can produce non-woven, medical, filtering material etc. enlarges its range of application;
2. the present invention adopts and adds in earlier stage in polymerization, guarantee metallic compound homodisperse in the nylon-6 matrix body, and give full play of metal-salt and the intermolecular interaction of nylon strengthening the modification ability, thereby make resin dedicated and spin denier/superfine denier nylon 6 long filaments.
3. the present invention adopts and adds metal salt compound before the polymerization, not only with the island method, peel off composite spinning method such as method and compare, technology is simple, cost reduces, and is a kind of eco-friendly high-performance fiber production technology; And utilize the master batch method to produce denier/superfine denier nylon 6 long filament technology before this with the contriver and compare, metal salt compound is good dispersity in nylon matrix, modifying function is more obvious, and technology is simplified more, reduced of the influence of spinning technique flow process to fibre property, make the gained fibre property stable, quality is more excellent; Simultaneously also reduce energy consumption, met the policy and the requirement of energy-saving and emission-reduction.
4. use special-purpose nylon 6 resins of the present invention and production method can obtain thin dawn or super fine denier nylon 6 fiber that fiber number is about 0.10～1.0dtex, the intensity of this fiber and elongation at break all meet the back requirements of weaving process, fill up the blank that domestic denier/superfine denier nylon 6 long filaments adopt conventional high speed spinning method to produce, promoted the scientific and technological content and the added value of nylon 6 fiber product.
Description of drawings
Fig. 1 is a Nylon 6 technological process of production synoptic diagram of the present invention.
Fig. 2 is the technological process of production synoptic diagram of nylon 6 long filaments of the present invention.
Embodiment
Below in conjunction with embodiment, be described more specifically content of the present invention.Should be appreciated that enforcement of the present invention is not limited to the following examples, all will fall into protection domain of the present invention any pro forma accommodation and/or the change that the present invention made.
In the present invention, if not refer in particular to, all equipment and raw material etc. all can be buied from market or the industry is commonly used.Method among the following embodiment if no special instructions, is the ordinary method of this area.
Main raw material:
Caprolactam monomer: Yueyang Ba Ling petrochemical industry company limited produces.
Embodiment 1:
As shown in Figure 1: above-mentioned materials is mixed in storage barrel, constantly above-mentioned material is sent in the straight type VK pipe by fresh feed pump, material is by the ring opening agent initiated polymerization, temperature control divides three phases in the described polyreaction, material is at straight type VK pipe epimere, and temperature is controlled between 230～260 ℃; Straight type VK pipe stage casing, temperature is controlled between 240～260 ℃; Straight type VK pipe hypomere, temperature is controlled between 220～240 ℃, and polymer melt is taken out of it by discharging pump through flowing to VK pipe bottom under the baffle plate layer by layer, and with liquid level in the holding tube, polymerization time is 10 hours.With the resulting polymers melt through the washing pelletizing, through vacuum-drying, to remove moisture and small-molecule substance.Drying temperature is at 90 ℃, and be 48 hours time of drying, promptly gets Nylon 6 of the present invention.
As shown in Figure 2: then the above-mentioned Nylon 6 that obtains is carried out melt-spinning, molten mass is delivered to spinning-drawing machine after extruding by screw extrusion press, quantitatively be pressed into molten mass in the spinning components through volume pump, by the orifice on the spinning jet nylon 6 melts are extruded with the filament attitude, again through cross air blow, cooling forming, oil boundling, hot drawing-off and coiling obtains fine denier nylon 6 fibrous finished products, wherein, melt screw extrusion press Zhong Ge district temperature be respectively 230 ℃, 250 ℃, 250 ℃, 255 ℃, spinning temperature is 250 ℃; 50 ℃ of hot drafting forming temperature, the spinning jet hole count of employing is 72, and the aperture is 0.35mm, and length is 0.7mm; Winding speed is 2000m/min, and by adjusting the volume pump rotating speed, obtaining the undrawn yarn fiber number is fine denier nylon 6 fibers of 0.9dtex, and Mechanics Performance Testing intensity reaches 3.4cN/dtex, and elongation at break is 120%.
Experiment shows, with the MgCl in the table 1
2Cl
-It is nitrogenous and/or contain oxygen and/or sulfur-bearing organic ligand or polynary part to replace to phosphate radical, carbonate, carboxylate radical, nitrate radical, sulfate radical, acetate, sulfonate radical, inferior sulfate radical, other halide anions, pseudohalogen ion and other, as porphyrin, thiocyanate ion, alanine root etc.; Distilled water replaces to deionized water; Hexanodioic acid replaces to the mixture of acetic acid or acetic acid and hexanodioic acid arbitrary proportion, can realize same technique effect, gives unnecessary details no longer one by one herein.
Embodiment 2:
As shown in Figure 1: above-mentioned materials is mixed in storage barrel, constantly above-mentioned material is sent in the straight type VK pipe by fresh feed pump, material is by the ring opening agent initiated polymerization, temperature control divides three phases in the described polyreaction, material is at straight type VK pipe epimere, and temperature is controlled between 230～275 ℃; Straight type VK pipe stage casing, temperature is controlled between 240～265 ℃; Straight type VK pipe hypomere, temperature is controlled between 220～245 ℃, and polymer melt is taken out of it by discharging pump through flowing to VK pipe bottom under the baffle plate layer by layer, and with liquid level in the holding tube, polymerization time is 14 hours.With the resulting polymers melt through the washing pelletizing, through vacuum-drying, to remove moisture and small-molecule substance.Drying temperature is at 90 ℃, and be 48 hours time of drying, promptly gets Nylon 6 of the present invention.
As shown in Figure 2: then the above-mentioned Nylon 6 that obtains is carried out melt-spinning, molten mass is delivered to spinning-drawing machine after extruding by screw extrusion press, quantitatively be pressed into molten mass in the spinning components through volume pump, by the orifice on the spinning jet nylon 6 melts are extruded with the filament attitude, again through cross air blow, cooling forming, oil boundling, hot drawing-off and coiling obtains fine denier nylon 6 fibrous finished products, wherein, melt screw extrusion press Zhong Ge district temperature be respectively 255 ℃, 265 ℃, 265 ℃, 268 ℃, spinning temperature is 260 ℃; 120 ℃ of hot drafting forming temperature, the spinning jet hole count of employing is 72, and the aperture is 0.35mm, and length is 0.7mm; Winding speed is 3000m/min, and by adjusting the volume pump rotating speed, obtaining the undrawn yarn fiber number is fine denier nylon 6 fibers of 0.8dtex, and Mechanics Performance Testing intensity reaches 3.6cN/dtex, and elongation at break is 95%.
Experiment shows, with the MgCl in the table 2
2Cl
-It is nitrogenous and/or contain oxygen and/or sulfur-bearing organic ligand or polynary part to replace to phosphate radical, carbonate, carboxylate radical, nitrate radical, sulfate radical, acetate, sulfonate radical, inferior sulfate radical, other halide anions, pseudohalogen ion and other, as porphyrin, thiocyanate ion, alanine root etc.; Distilled water replaces to deionized water; Hexanodioic acid replaces to the mixture of acetic acid or acetic acid and hexanodioic acid arbitrary proportion, can realize same technique effect, gives unnecessary details no longer one by one herein.
Embodiment 3:
As shown in Figure 1: above-mentioned materials is mixed in storage barrel, constantly above-mentioned material is sent in the straight type VK pipe by fresh feed pump, material is by the ring opening agent initiated polymerization, temperature control divides three phases in the described polyreaction, material is at straight type VK pipe epimere, and temperature is controlled between 230～270 ℃; Straight type VK pipe stage casing, temperature is controlled between 240～260 ℃; Straight type VK pipe hypomere, temperature is controlled between 235～260 ℃, and polymer melt is taken out of it by discharging pump through flowing to VK pipe bottom under the baffle plate layer by layer, and with liquid level in the holding tube, polymerization time is 16 hours.With the resulting polymers melt through the washing pelletizing, through vacuum-drying, to remove moisture and small-molecule substance.Drying temperature is at 100 ℃, and be 24 hours time of drying, promptly gets Nylon 6 of the present invention.
As shown in Figure 2: then the above-mentioned Nylon 6 that obtains is carried out melt-spinning, molten mass is delivered to spinning-drawing machine after extruding by screw extrusion press, quantitatively be pressed into molten mass in the spinning components through volume pump, by the orifice on the spinning jet nylon 6 melts are extruded with the filament attitude, again through cross air blow, cooling forming, oil boundling, hot drawing-off and coiling obtains fine denier nylon 6 fibrous finished products, wherein, melt screw extrusion press Zhong Ge district temperature be respectively 260 ℃, 272 ℃, 272 ℃, 273 ℃, spinning temperature is 260 ℃; 130 ℃ of hot drafting forming temperature, the spinning jet hole count of employing is 10, and the aperture is 0.3mm, and length is 1.0mm; Winding speed is 4000m/min, and by adjusting the volume pump rotating speed, obtaining the undrawn yarn fiber number is fine denier nylon 6 fibers of 0.7dtex, and Mechanics Performance Testing intensity reaches 4.3cN/dtex, elongation at break 65%.
Experiment shows, with the Ca in the table 3 (Ac)
2Ac
-It is nitrogenous and/or contain oxygen and/or sulfur-bearing organic ligand or polynary part to replace to phosphate radical, carbonate, nitrate radical, sulfate radical, sulfonate radical, inferior sulfate radical, other halide anions, pseudohalogen ion and other, as porphyrin, thiocyanate ion, alanine root etc.; Distilled water replaces to deionized water; Hexanodioic acid replaces to the mixture of acetic acid or acetic acid and hexanodioic acid arbitrary proportion, can realize same technique effect, gives unnecessary details no longer one by one herein.
Embodiment 4
As shown in Figure 1: above-mentioned materials is mixed in storage barrel, constantly above-mentioned material is sent in the straight type VK pipe by fresh feed pump, material is by the ring opening agent initiated polymerization, temperature control divides three phases in the described polyreaction, material is at straight type VK pipe epimere, and temperature is controlled between 230～275 ℃; Straight type VK pipe stage casing, temperature is controlled between 245～265 ℃; Straight type VK pipe hypomere, temperature is controlled between 230～260 ℃, and polymer melt is taken out of it by discharging pump through flowing to VK pipe bottom under the baffle plate layer by layer, and with liquid level in the holding tube, polymerization time is 18 hours.With the resulting polymers melt through the washing pelletizing, through vacuum-drying, to remove moisture and small-molecule substance.Drying temperature is at 95 ℃, and be 30 hours time of drying, promptly gets Nylon 6 of the present invention.
As shown in Figure 2: then the above-mentioned Nylon 6 that obtains is carried out melt-spinning, molten mass is delivered to spinning-drawing machine after extruding by screw extrusion press, quantitatively be pressed into molten mass in the spinning components through volume pump, by the orifice on the spinning jet nylon 6 melts are extruded with the filament attitude, again through cross air blow, cooling forming, oil boundling, hot drawing-off and coiling obtains super fine denier nylon 6 fiber finished product, wherein, melt screw extrusion press Zhong Ge district temperature be respectively 260 ℃, 273 ℃, 273 ℃, 277 ℃, spinning temperature is 275 ℃; 155 ℃ of hot drafting forming temperature, the spinning jet hole count of employing is 24, and the aperture is 0.2mm, and length is 0.6mm; Winding speed is 4500m/min, and by adjusting the volume pump rotating speed, obtaining the undrawn yarn fiber number is the super fine denier nylon 6 fiber of 0.5dtex, and Mechanics Performance Testing intensity reaches 4.8cN/dtex, elongation at break 45%.
Experiment shows, with the CaCl in the table 4
2Cl
-It is nitrogenous and/or contain oxygen and/or sulfur-bearing organic ligand or polynary part to replace to phosphate radical, carbonate, carboxylate radical, nitrate radical, sulfate radical, acetate, sulfonate radical, inferior sulfate radical, other halide anions, pseudohalogen ion and other, as porphyrin, thiocyanate ion, alanine root etc.; Distilled water replaces to deionized water; Hexanodioic acid replaces to the mixture of acetic acid or acetic acid and hexanodioic acid arbitrary proportion, can realize same technique effect, gives unnecessary details no longer one by one herein.
Embodiment 5
As shown in Figure 1: above-mentioned materials is mixed in storage barrel, constantly above-mentioned material is sent in the straight type VK pipe by fresh feed pump, material is by the ring opening agent initiated polymerization, temperature control divides three phases in the described polyreaction, material is at straight type VK pipe epimere, and temperature is controlled between 230～290 ℃; Straight type VK pipe stage casing, temperature is controlled between 240～280 ℃; Straight type VK pipe hypomere, temperature is controlled between 240～270 ℃, and polymer melt is taken out of it by discharging pump through flowing to VK pipe bottom under the baffle plate layer by layer, and with liquid level in the holding tube, polymerization time is 20 hours.With the resulting polymers melt through the washing pelletizing, through vacuum-drying, to remove moisture and small-molecule substance.Drying temperature is at 95 ℃, and be 30 hours time of drying, promptly gets Nylon 6 of the present invention.
As shown in Figure 2: then the above-mentioned Nylon 6 that obtains is carried out melt-spinning, molten mass is delivered to spinning-drawing machine after extruding by screw extrusion press, quantitatively be pressed into molten mass in the spinning components through volume pump, by the orifice on the spinning jet nylon 6 melts are extruded with the filament attitude, again through cross air blow, cooling forming, oil boundling, hot drawing-off and coiling obtains super fine denier nylon 6 fiber finished product, wherein, melt screw extrusion press Zhong Ge district temperature be respectively 265 ℃, 278 ℃, 278 ℃, 280 ℃, spinning temperature is 280 ℃; 170 ℃ of hot drafting forming temperature, the spinning jet hole count of employing is 48, and the aperture is 0.1mm, and length is 0.4mm; Winding speed is 6000m/min, and by adjusting the volume pump rotating speed, obtaining the undrawn yarn fiber number is the super fine denier nylon 6 fiber of 0.20dtex, and Mechanics Performance Testing intensity reaches 5.3cN/dtex, elongation at break 34%.
Experiment shows, with the CaCl in the table 5
2Cl
-It is nitrogenous and/or contain oxygen and/or sulfur-bearing organic ligand or polynary part to replace to phosphate radical, carbonate, carboxylate radical, nitrate radical, sulfate radical, acetate, sulfonate radical, inferior sulfate radical, other halide anions, pseudohalogen ion and other, as porphyrin, thiocyanate ion, alanine root etc., distilled water replaces to deionized water; Hexanodioic acid replaces to the mixture of acetic acid or acetic acid and hexanodioic acid arbitrary proportion, can realize same technique effect, gives unnecessary details no longer one by one herein.
Embodiment 6
As shown in Figure 1: above-mentioned materials is mixed in storage barrel, constantly above-mentioned material is sent in the straight type VK pipe by fresh feed pump, material is by the ring opening agent initiated polymerization, temperature control divides three phases in the described polyreaction, material is at straight type VK pipe epimere, and temperature is controlled between 250～300 ℃; Straight type VK pipe stage casing, temperature is controlled between 260～290 ℃; Straight type VK pipe hypomere, temperature is controlled between 240～270 ℃, and polymer melt is taken out of it by discharging pump through flowing to VK pipe bottom under the baffle plate layer by layer, and with liquid level in the holding tube, polymerization time is 16 hours.With the resulting polymers melt through the washing pelletizing, through vacuum-drying, to remove moisture and small-molecule substance.Drying temperature is at 92 ℃, and be 36 hours time of drying, promptly gets Nylon 6 of the present invention.
As shown in Figure 2: then the above-mentioned Nylon 6 that obtains is carried out melt-spinning, molten mass is delivered to spinning-drawing machine after extruding by screw extrusion press, quantitatively be pressed into molten mass in the spinning components through volume pump, by the orifice on the spinning jet nylon 6 melts are extruded with the filament attitude, again through cross air blow, cooling forming, oil boundling, hot drawing-off and coiling obtains fine denier nylon 6 fibrous finished products, wherein, melt screw extrusion press Zhong Ge district temperature be respectively 265 ℃, 270 ℃, 270 ℃, 273 ℃, spinning temperature is 268 ℃; 140 ℃ of hot drafting forming temperature, the spinning jet hole count of employing is 150, and the aperture is 0.6mm, and length is 1.2mm; Winding speed is 4000m/min, and by adjusting the volume pump rotating speed, obtaining the undrawn yarn fiber number is fine denier nylon 6 fibers of 0.9dtex, and Mechanics Performance Testing intensity reaches 4.4cN/dtex, elongation at break 40%.
Experiment shows, with Sr in the table 6 (SCN)
2SCN
-It is nitrogenous and/or contain oxygen and/or sulfur-bearing organic ligand or polynary part to replace to phosphate radical, carbonate, carboxylate radical, nitrate radical, sulfate radical, sulfonate radical, inferior sulfate radical, halide anion, pseudohalogen ion and other, as porphyrin, alanine root etc., distilled water replaces to deionized water; Hexanodioic acid replaces to the mixture of acetic acid or acetic acid and hexanodioic acid arbitrary proportion, can realize same technique effect, gives unnecessary details no longer one by one herein.
Above preferred embodiment just is used for description and interpretation content of the present invention, does not constitute the restriction to content of the present invention.Although the contriver has done in more detail the present invention and has enumerated, but, the content that those skilled in the art is disclosed according to summary of the invention part and embodiment, can make various modifications or/and to replenish or adopt similar mode to substitute be obvious to described specific embodiment, and can realize technique effect of the present invention, therefore, give unnecessary details no longer one by one herein.The term that occurs among the present invention is used for the elaboration of technical solution of the present invention and understanding are not construed as limiting the invention.
Claims (9)
1. Nylon 6, it is characterized in that described Nylon 6 is that the blend melt by the compound of the caprolactam monomer and second main group metal makes through polyreaction, wherein, based on caprolactam monomer gross weight meter, the weight of the compound of second main group metal is 0.01～1.0%.
2. a kind of Nylon 6 according to claim 1, it is characterized in that, the compound of described second main group metal is second main group metal salt or the complex compound, wherein, described second main group metal is selected from magnesium, calcium or strontium, and it is nitrogenous and/or contain oxygen and/or sulfur-bearing organic ligand or polynary part that the negatively charged ion of the described second main group metal salt or the part of complex compound are selected from hydroxide radical, phosphate radical, carbonate, carboxylate radical, nitrate radical, sulfate radical, acetate, sulfonate radical, inferior sulfate radical, halide anion, pseudohalogen ion and other.
3. a kind of Nylon 6 according to claim 1, it is characterized in that, add ring opening agent and molecular weight stabilizer in the described polyreaction, wherein, described ring opening agent is meant distilled water or deionized water, and the addition of ring opening agent accounts for 1～5% of caprolactam monomer gross weight; Described molecular weight stabilizer is meant acetic acid or/and hexanodioic acid, and the addition of molecular weight stabilizer accounts for 0.1～0.5% of caprolactam monomer gross weight.
4. a kind of Nylon 6 according to claim 1 is characterized in that, in the described polyreaction: temperature control divides three phases, and material is at the straight type successive polymerization of normal pressure pipe epimere, and temperature is controlled between 230～300 ℃; In straight type VK pipe stage casing, temperature is controlled between 240～290 ℃; At straight type VK pipe hypomere, temperature is controlled between 220～270 ℃; Polymerization time is 10-20h.
5. one kind by the nylon 6 fiber of the arbitrary described Nylon 6 of claim 1-4 through melt spinning method preparation.
6. nylon 6 fiber according to claim 5 is characterized in that, the fiber number of described nylon 6 fiber is 0.1～1.0dtex.
7. the preparation method of a nylon 6 fiber as claimed in claim 5 is characterized in that, described preparation method comprises: Nylon 6 is carried out melt-spinning, and wherein, in the melt-spinning process: the temperature of nylon 6 molten masses is between 130～320 ℃; The hole count of spinning jet is 10～150, and the aperture is 0.1～0.6mm, and the spinning jet length-to-diameter ratio is 2.0～4.0; The speed of reeling is 2000～6000m/min.
8. the preparation method of nylon 6 fiber according to claim 7 is characterized in that, before the described melt-spinning Nylon 6 is carried out drying, and drying temperature is 90-100 ℃, and be 24-48 hour time of drying.
9. the preparation method of nylon 6 fiber according to claim 7 is characterized in that, also does hot drawing-off before the described coiling, and the temperature of hot drawing-off is between 50-170 ℃.
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| CN103845955A (en) * | 2012-12-03 | 2014-06-11 | 北京大学 | Fine denier nylon filter cloth, preparation method and applications thereof |
| CN103845954A (en) * | 2012-12-03 | 2014-06-11 | 北京大学 | Novel weaving method of nylon filter cloth, filter cloth weaved through the weaving method, and application of the filter cloth |
| CN104562250A (en) * | 2014-11-27 | 2015-04-29 | 杭州师范大学 | Micro-porous fine denier nylon 6 three-difference fiber and preparation method and application thereof |
| CN112501812A (en) * | 2020-11-05 | 2021-03-16 | 江苏文明人造草坪有限公司 | Artificial turf with high single-cluster pull-out force and preparation process thereof |
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| CN101139748A (en) * | 2007-07-13 | 2008-03-12 | 杭州师范大学 | Fine denier or ultra-fine denier nylon fibre and production method thereof |
| CN101148506A (en) * | 2007-11-02 | 2008-03-26 | 湖南大学 | Method for producing high-fluidity nylon 6 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101139748A (en) * | 2007-07-13 | 2008-03-12 | 杭州师范大学 | Fine denier or ultra-fine denier nylon fibre and production method thereof |
| CN101148506A (en) * | 2007-11-02 | 2008-03-26 | 湖南大学 | Method for producing high-fluidity nylon 6 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103845955A (en) * | 2012-12-03 | 2014-06-11 | 北京大学 | Fine denier nylon filter cloth, preparation method and applications thereof |
| CN103845954A (en) * | 2012-12-03 | 2014-06-11 | 北京大学 | Novel weaving method of nylon filter cloth, filter cloth weaved through the weaving method, and application of the filter cloth |
| CN103845954B (en) * | 2012-12-03 | 2016-04-27 | 北京大学 | The new weave of nylon filtering cloth, filter cloth of being made into thus and uses thereof |
| CN103845955B (en) * | 2012-12-03 | 2016-04-27 | 北京大学 | Fine denier nylon filter cloth, Preparation Method And The Use |
| CN104562250A (en) * | 2014-11-27 | 2015-04-29 | 杭州师范大学 | Micro-porous fine denier nylon 6 three-difference fiber and preparation method and application thereof |
| CN112501812A (en) * | 2020-11-05 | 2021-03-16 | 江苏文明人造草坪有限公司 | Artificial turf with high single-cluster pull-out force and preparation process thereof |
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