CN103966673A

CN103966673A - Fine-denier nylon raw material blend spinning masterbatch

Info

Publication number: CN103966673A
Application number: CN201410039182.3A
Authority: CN
Inventors: 刘毓海; 高云龙; 高苑; 刘少轩; 陈静; 刘俊; 贺安琪; 杨展澜; 徐怡庄; 吴瑾光
Original assignee: Peking University
Current assignee: Peking University
Priority date: 2013-01-29
Filing date: 2014-01-27
Publication date: 2014-08-06
Anticipated expiration: 2034-01-27
Also published as: CN103966673B

Abstract

The invention discloses fine-denier nylon raw material blend spinning masterbatch which is formed by nylon smashing and pressurizing. Nylon is smashed into powder and is mixed with melt spinning additive powder, main materials are obtained, the main materials are subjected to pressurizing forming, and components such as dispersing agents, binding agents, disintegrating agents, hydrotropy agents, lubricating agents and coating agents are randomly added during the pressurizing-forming process. According to the masterbatch, the effective concentration of melt spinning additives and auxiliary materials in the blend spinning masterbatch can be obviously improved, various components of the blend spinning masterbatch are evenly dispersed, component varieties and content can be easily controlled, high-temperature operation is of no need, and producing/processing/preparing processes are safe.

Description

Fine denier nylon raw material blending spinning master batch

Technical Field

The invention relates to a textile technology, in particular to a raw material blending spinning master batch for producing fine denier nylon (fiber).

Background

In general, the spinnable polymer material includes natural fiber and chemical fiber. Wherein the chemical fiber mainly comprises: polyamide (commonly known as "chinlon" or "nylon"), polypropylene (commonly known as "polypropylene"), polyethylene terephthalate (commonly known as "polyester"), polyacrylonitrile (commonly known as "acrylon"), and the like. These materials can be spun to form filaments for use in the textile industry, where melt spinning is a common spinning technique by which filaments suitable for textile use can be obtained.

Among them, nylon is the earliest synthetic fiber in the world, and is characterized by high strength and good wear resistance, and the strength and wear resistance of nylon are the first of all fibers. Nylon has the same disadvantages and deficiencies as other chemical fibers, such as poor softness, poor moisture absorption and permeability, and the like.

With the increasing living standard of people, the requirements for the properties of nylon fiber textiles are higher and higher, such as softness, hygroscopicity, dyeability, antistatic property, flame resistance, stain resistance, anti-pilling property and the like, so scientists use chemical or physical methods to improve the properties of nylon fibers, such as moisture absorption, dyeing, antistatic property, flame resistance, stain resistance, anti-pilling property and the like, by changing the structure of a chemical fiber polymerization monomer or changing the denier of the fibers.

Research shows that the characteristics of softness, hygroscopicity, uniformity, strength and the like of the fiber are inversely proportional to the thickness of the fiber, and the thickness of the fiber is measured by denier, namely the mass of the fiber per unit length is in dtex, so that high-performance and new-variety fine-denier nylon fibers are usually realized by reducing the denier of the nylon fibers, the reduction of the denier of the nylon is usually realized by adding additives and auxiliary materials which play roles in modifying, reducing defects, improving performance and the like into a nylon raw material in a melt spinning process, and the addition amount and the uniformity of the additives and the auxiliary materials play a key role in the nylon modification result.

The traditional method for adding additives and auxiliary materials mainly comprises the following two methods: direct addition method and master batch addition method. The direct addition method is that various additives and auxiliary materials are directly added into nylon spinning raw materials in a melt spinning link to prepare a spinning melt, and nylon fibers are prepared; the master batch adding method is that various additives and auxiliary materials are mixed with a small amount of nylon spinning raw materials before the melt spinning link to prepare blended spinning master batches, and then the prepared blended spinning master batches are put into a large amount of nylon spinning raw materials in the melt spinning link to prepare the nylon fibers.

The direct addition method has the following disadvantages although the steps are simple: the addition of the additive/auxiliary material is uneven, the aggregation is obvious, and the uniformity of the product is poor; the addition amount is difficult to control, accurate quantitative addition is difficult to realize, and the proportion of each additive is difficult to be constant, so that the product quality is unstable; the concentrated addition of chemically active additives may cause damage to the production equipment.

Compared with the prior art, the master batch adding method has the advantages of constant proportion of various additives, easy control of the addition amount of the spinning master batch, uniform dispersion, no damage to production equipment and the like, thereby effectively ensuring the stability of the quality of spinning products, and therefore, most of high-performance and new-variety fibers are synthesized by adopting the master batch adding method.

At present, spinning master batches used for a master batch addition method are basically prepared by a hot melt blending mode, namely, a small amount of nylon spinning raw materials are melted to form a nylon spinning raw material melt before a melt spinning link, the nylon spinning raw material melt and various auxiliary materials are fully stirred, blended and sheared, and finally cooled to obtain the spinning master batches. The spinning master batch is prepared by adopting the method, the nylon spinning raw material in the spinning master batch needs to be subjected to a high-temperature melting stage, a large amount of energy is consumed, the problems of nylon thermal degradation and the like are caused frequently, and meanwhile, in order to keep the fluidity of the molten spinning master batch raw material in the spinning master batch production process, the concentration of various auxiliary materials in the spinning master batch is limited, so that the performance optimization of a spinning product is limited.

Therefore, it is very important to develop a new generation of spinning masterbatch with low cost and low energy consumption.

Disclosure of Invention

In order to solve the above problems, the present inventors have conducted extensive studies and experiments, and as a result, found that: the spinning master batch prepared by the method can effectively improve the effective concentration and the uniformity of the melt spinning additive and the auxiliary material in the spinning master batch, and the preparation process does not pass through the high-temperature melting process, so that the thermal degradation of the nylon raw material can be effectively avoided, and the spinning master batch with higher efficiency and higher quality can be obtained compared with the existing hot melt blending mode.

The invention aims to provide the following aspects:

in a first aspect, the present invention provides a fine denier nylon raw material blended spinning masterbatch, which is characterized in that the blended spinning masterbatch comprises:

(1) the master batch comprises the following main materials: nylon and a melt spinning additive, wherein the weight ratio of the nylon to the melt spinning additive is 1: 10-10: 1;

the nylon comprises nylon 6, nylon 66, nylon 10, nylon 12, nylon 1212 and nylon 610;

the melt spinning additive is selected from the group consisting of compounds or complexes formed from cations and anions of the following metals,

the metal is selected from:

magnesium, calcium, strontium, aluminum, gallium, indium, germanium, tin, bismuth, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, zirconium, molybdenum, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, and lutetium;

the anion is selected from: phosphates, carbonates, carboxylates, nitrates, sulfates, sulfonates, sulfites, halogen anions, pseudohalogen ions and other nitrogen-and/or oxygen-and/or sulfur-containing organic ligands or polyligands, as well as derivatives of the foregoing;

(2) the auxiliary material is at least one of dispersant, adhesive, disintegrant, cosolvent, lubricant and coating agent;

wherein,

the dispersant is selected from: hexenyl bis stearamide, glyceryl monostearate, glyceryl tristearate, hydrocarbon waxes or mixtures thereof; barium stearate, zinc stearate, calcium stearate, cadmium stearate, magnesium stearate or copper stearate; ethylene-acrylic acid copolymer, ethylene-vinyl acetate copolymer or polyethylene wax;

the adhesive is selected from: starch, protein, dextrin, animal glue, shellac, hide glue or rosin; asphalt; water glass; polyethylene, polypropylene, polystyrene, polyvinyl chloride, silicone rubber, fluororubber, polysulfide rubber, chlorohydrin rubber, nitrile rubber, polyacrylate rubber, urethane rubber, or butyl rubber; polyvinyl alcohol, carboxymethyl cellulose, polyurethane, polystyrene, polyacrylate, ethylene-vinyl acetate copolymer, butyl rubber, vinyl resin, acrylic resin, chlorinated rubber, epoxy resin, silicone oil and dimethyl silicone oil are used singly or in a mixture;

the disintegrant is selected from: dry starch, sodium carboxymethyl starch; low-substituted hydroxypropyl cellulose, effervescent disintegrant, crospovidone or croscarmellose sodium;

the cosolvent is selected from: sodium benzoate, sodium salicylate, p-aminobenzoic acid; urea, nicotinamide or acetamide; borax or potassium iodide;

the lubricant is selected from: mechanical oil, loom oil, main shaft oil, rail oil, steel rolling oil, gas turbine oil, compressor oil, refrigerator oil, cylinder oil, marine oil, gear oil, machine pressure gear oil, axle oil, instrument oil and vacuum pump oil; castor oil or tallow; silicone oil, fatty acid amide, oleic acid, polyester, synthetic ester, or carboxylic acid; graphite, molybdenum disulfide, polytetrafluoroethylene, nylon, boron nitride, or graphite fluoride;

the coating agent is selected from: hydroxypropyl methylcellulose, hydroxypropyl cellulose, acrylic resin IV, polyvinylpyrrolidone, cellulose acetate phthalate, hydroxypropyl methylcellulose phthalate, polyvinyl alcohol phthalate, styrene maleic acid copolymer, acrylic resin, ethyl cellulose, cellulose acetate, hydroxypropyl cellulose, hypromellose, microcrystalline cellulose, povidone, polyethylene glycol, or polyvinyl alcohol;

wherein the weight ratio of the master batch main material to the auxiliary material is 1: 1-100: 0.5.

In a second aspect, the invention provides the fine denier nylon raw material blending spinning master batch, which is characterized in that the weight ratio of the nylon powder to the melt spinning additive is 1: 3-3: 1.

The third aspect of the invention provides the fine denier nylon raw material blending spinning master batch, which is characterized in that the weight ratio of the master batch main material to the auxiliary material is 10: 1-100: 2.

In a fourth aspect, the invention provides the fine denier nylon raw material blending spinning master batch, which is characterized in that the dispersing agent is glyceryl tristearate.

In a fifth aspect, the invention provides the fine denier nylon raw material blended spinning masterbatch, which is characterized in that the adhesive is acrylic resin.

In a sixth aspect, the invention provides the fine denier nylon raw material blended spinning masterbatch, which is characterized in that the disintegrant is dry starch.

In a seventh aspect, the invention provides the fine denier nylon raw material blending spinning masterbatch, which is characterized in that the cosolvent is selected from sodium benzoate or borax.

In an eighth aspect, the invention provides the fine denier nylon raw material blended spinning masterbatch, wherein the lubricant is selected from silicone oil or graphite fluoride.

In a ninth aspect, the invention provides the fine denier nylon raw material blended spinning masterbatch, wherein the coating agent is selected from hydroxypropyl methyl cellulose or hydroxypropyl cellulose, and the coating agent is used alone or in combination.

In a tenth aspect, the invention provides the fine denier nylon raw material blended spinning masterbatch, which is characterized in that the blended spinning masterbatch is prepared by the following steps:

A. nylon crushing: crushing nylon particles at the temperature of-200-100 ℃ to obtain nylon powder with the diameter of less than 5 mu m, mixing the prepared nylon powder and a melt spinning additive according to the weight ratio of 1: 10-10: 1 at normal temperature and normal pressure, and uniformly stirring to obtain a master batch;

B. and (3) pressure forming: fully mixing the master batch prepared in the step A and the auxiliary materials according to the weight ratio of 1: 1-100: 0.5 at normal temperature and normal pressure to obtain a blending master batch raw material; and pressurizing the prepared blending master batch raw material at the temperature of 0-200 ℃ and the pressure of 0.1-10 MPa to prepare the blending spinning master batch.

The melt spinning method is characterized in that raw materials for spinning are heated and melted, a melt is extruded by a screw extruder and then sent to a spinning machine, the melt is quantitatively pressed into a spinning part by a metering pump, a nylon melt is extruded in a filament state through a spinneret orifice on a spinneret plate, a finished product is obtained by cooling and forming after cross air blowing, oiling, bundling and winding are carried out, or the finished product is obtained by hot drawing after the oiling, bundling is carried out, and fine denier nylon filaments are obtained.

In the method of the present invention, the term "pressure forming" means that nylon, melt spinning additives and other auxiliary materials are pressed into a desired shape by means of mechanical pressing.

The term "melt spinning additive" as used in the process of the present invention means a substance which is added to the nylon raw material in a small amount during the melt spinning process, and which can significantly improve the fiber properties or impart to the nylon spun product some new properties not exhibited by the raw nylon spun product.

In the method of the invention, the term "auxiliary material" is used to refer to an additive which is not used for improving the fiber performance, but is used for increasing the molding, disintegration and other performances of the blended spinning master batch.

The fine denier nylon raw material blending spinning master batch provided by the invention has the following advantages:

(1) the effective concentration of the melt spinning additive and the auxiliary material in the blended spinning master batch is obviously improved;

(2) the types and the contents of various additives and auxiliary materials in the blended spinning master batch are easier to control, and all components are uniformly dispersed;

(3) the blended spinning master batch has uniform size, is convenient to package, and can realize accurate and quantitative addition of the blended spinning master batch in the subsequent melt spinning process;

(4) the preparation process of the blended spinning master batch does not have a high-temperature melting process, so that the thermal degradation of nylon is effectively avoided, and the quality of the spun nylon fiber is ensured;

(5) the preparation process of the blended spinning master batch does not need high-temperature operation, reduces energy consumption, is green and environment-friendly, reduces production cost, and simultaneously ensures that the production, processing and preparation processes are safer and more reliable.

Detailed Description

The invention is further described below by means of specific examples. The features and advantages of the present invention will become more apparent as the description proceeds. However, these examples are merely illustrative for explaining the present invention, and do not set any limit to the scope of the present invention. It will be understood by those skilled in the art that the present invention may be modified and/or changed in detail and/or substituted with equivalents without departing from the spirit and scope of the invention, and that such modifications/changes/substitutions are intended to be within the scope of the invention as claimed.

The invention provides fine denier nylon raw material blending spinning master batch, which comprises the following components:

(1) the master batch comprises the following main materials: nylon and a melt spinning additive in a weight ratio of 1:10 to 10:1, wherein,

the melt spinning additive is a main substance which plays a role in modification in the melt spinning process, and optimizes the performance of the prepared fiber, such as the strength, elongation at break, water absorption, softness and the like of the fiber filament, by utilizing the chemical properties of the melt spinning additive in the subsequent spinning process, wherein the metal is selected from magnesium, calcium, strontium, aluminum, gallium, indium, germanium, tin, bismuth, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, zirconium, molybdenum, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium; the ligand of the anion or complex is selected from: phosphates, carbonates, carboxylates, nitrates, sulfates, sulfonates, sulfites, halogen anions, pseudohalogen ions and other nitrogen-and/or oxygen-and/or sulfur-containing organic ligands or polyligands, as well as derivatives of the foregoing; the properties of nylon fibers can be improved with a single component or a mixture of compounds consisting of the above anions and cations.

in the spinning process, the more uniformly the melt spinning additive is dispersed in the nylon raw material, the better the modification effect on nylon is, so that the quality of the prepared nylon fiber is better, therefore, organic polymers or inorganic salts which can play a role in dispersion are usually added, the dispersing agent can uniformly disperse master batch main materials into the nylon raw material in the melt spinning process, so that the melt spinning additive and the nylon raw material are fully and uniformly mixed, and therefore, a substance which can be mutually dissolved with the nylon raw material or a substance with good dispersion degree in the nylon raw material is selected, and the dispersing agent selected by the invention is selected from: hexenyl bis stearamide (EBS), Glyceryl Monostearate (GMS), glyceryl tristearate (HTG), hydrocarbon paraffin solids and the like, alone or in combination; liquid paraffin or microcrystalline paraffin; barium stearate, zinc stearate, calcium stearate, cadmium stearate, magnesium stearate or copper stearate; ethylene-acrylic acid copolymer, ethylene-vinyl acetate copolymer or polyethylene wax (PEG), preferably glyceryl tristearate (HTG).

When the blended spinning master batch is prepared, the blended spinning master batch main material is difficult to achieve certain hardness by only mechanically pressurizing, so that an adhesive needs to be added into the master batch main material to ensure that the master batch main material has viscosity, and is convenient for subsequent pressure forming, and the method comprises the following steps: starch, protein, dextrin, animal glue, shellac, hide glue or rosin; asphalt; water glass; polyethylene, polypropylene, polystyrene, polyvinyl chloride, silicone rubber, fluororubber, polysulfide rubber, chlorohydrin rubber, nitrile rubber, polyacrylate rubber, urethane rubber, or butyl rubber; polyvinyl alcohol, carboxymethyl cellulose, polyurethane, polystyrene, polyacrylate, ethylene-vinyl acetate copolymer, butyl rubber, vinyl resin, acrylic resin, chlorinated rubber, epoxy resin, silicone oil or dimethyl silicone oil are used alone or in combination, and acrylic resin is preferred.

In order to ensure that the blended spinning master batch is successfully disintegrated in the nylon raw material to release the melt spinning additive, the disintegrating agent is selected from: dry starch or sodium carboxymethyl starch (CMS-Na); low substituted hydroxypropyl cellulose (L-HPC), effervescent disintegrant, crospovidone, or croscarmellose sodium (CCNa).

In the melt spinning process, the cosolvent has the function of dissolving the melt spinning additive released by disintegration in the blended spinning master batch more fully in the molten nylon raw material so as to modify the molten nylon raw material, and the cosolvent used in the invention is selected from: sodium benzoate, sodium salicylate or p-aminobenzoic acid; urea, nicotinamide or acetamide; borax or potassium iodide.

In the process of preparing the blended spinning master batch by pressurization, the lubricant can play a role in increasing the fluidity of the blended spinning master batch raw material in the compression molding/tabletting process, thereby improving the efficiency of the pressurization molding. Animal or vegetable oils are good natural lubricants; synthetic oils can perform the same function because they also have a similar structure to natural oils; some inorganic substances with a phosphorus layer structure, such as graphite fluoride, can also play a role in lubrication, so that the lubricant used in the invention is selected from the following: mechanical oil, loom oil, main shaft oil, rail oil, steel rolling oil, gas turbine oil, compressor oil, refrigerator oil, cylinder oil, marine oil, gear oil, machine pressure gear oil, axle oil, instrument oil or vacuum pump oil; castor oil or tallow; silicone oil, fatty acid amide, oleic acid, polyester, synthetic ester, or carboxylic acid; graphite, molybdenum disulfide, polytetrafluoroethylene, nylon, boron nitride or graphite fluoride, preferably silicone oil or graphite fluoride.

In order to make the blended spinning master batch product after pressure forming easy to demould, in the process of preparing the blended spinning master batch by pressure, a substance with small viscosity force with a mould, namely a coating agent, needs to be added, so that the blended spinning master batch keeps a good shape in the demoulding process, and the coating agent selected by the invention is selected from the following components: hydroxypropyl methylcellulose (HPMC), hydroxypropyl cellulose (HPC), acrylic resin IV or polyvinylpyrrolidone (PVP), Cellulose Acetate Phthalate (CAP), hydroxypropyl methylcellulose phthalate (HPMCP), polyvinyl alcohol phthalate (PVAP), styrene maleic acid copolymer (StyMA), acrylic resin, ethyl cellulose, cellulose acetate, hydroxypropyl cellulose, hypromellose, microcrystalline cellulose, povidone, polyethylene glycol, or polyvinyl alcohol, and preferably, hydroxypropyl methylcellulose or hydroxypropyl cellulose, alone or in combination.

The blending spinning master batch has the effects that the blending spinning master batch is disintegrated in a molten nylon raw material during melt spinning, so that a melt spinning additive in the nylon raw material is added into the nylon raw material, the nylon raw material is modified, in order to enable the melt spinning additive to be added into the nylon raw material more uniformly, the local concentration of the melt spinning additive in the melt nylon raw material needs to be controlled not to be too high, otherwise, the quality of the prepared nylon fiber is easily uneven, so that the performance of nylon is reduced, and the weight ratio of nylon powder to the melt spinning additive is controlled not to be more than 10: 1; the amount of the melt spinning additive added into the nylon raw material can be adjusted by the amount of the blended spinning master batch, the content of the additive cannot be too low, and excessive auxiliary materials are prevented from being introduced into the nylon raw material, so that the performance of the nylon fiber is reduced, and therefore, the weight ratio of the nylon powder to the melt spinning additive is controlled to be not less than 1: 10.

The blended spinning master batch provided by the invention is prepared by the following steps:

A. nylon crushing: crushing nylon particles at-200-100 ℃, preferably-200-10 ℃ to obtain nylon powder with the diameter of less than 5 mu m, mixing the prepared nylon powder and a melt spinning additive according to the weight ratio of 1: 10-10: 1 at normal temperature and normal pressure, and uniformly stirring to obtain a master batch;

In the step A, in order to prevent the nylon raw material and the melt spinning additive from being melted due to frictional heat generation in the nylon crushing process, so that the nylon powder and the melt spinning additive are not uniformly mixed and have poor formability, a cooling device such as a liquid nitrogen cooling device is selected to enable nylon particles to be in a low-temperature environment to form nylon powder with good dispersibility, so that the nylon powder is convenient to be mixed with the melt spinning additive and subjected to pressure forming subsequently, and the temperature is controlled to be-200-100 ℃ due to the fact that the melting point ranges of different types of nylon are 200-300 ℃.

Because the nylon blended spinning master batch provided by the invention is prepared by adopting a cold pressing method, namely nylon powder is directly mixed with a melt spinning additive and auxiliary materials at normal temperature and normal pressure, and then the blended spinning master batch is directly formed by mechanical pressurization, without high temperature melting process, the particle size of the nylon powder and the degree of proximity to the particle size of the melt spinning additive/auxiliary material directly influence the mixing uniformity of the nylon powder, the melt spinning additive and the auxiliary material in the blended spinning master batch and the molding effect of the blended spinning master batch, the uniform degree of mixing of all components in the blended spinning master batch directly influences the dispersion degree of the blended spinning master batch in a molten nylon raw material in a melt spinning process, the more uniformly the nylon powder is mixed with the melt spinning additive/auxiliary material, the better the dispersion degree of the nylon fiber in a molten state in the nylon raw material, the better the quality of the prepared nylon fiber; meanwhile, the more uniformly the nylon powder is mixed with various additives/auxiliary materials, the easier the operation is in preparing the blended spinning master batch, and the easier the prepared blended spinning master batch is formed; the grain diameter of the additive and the auxiliary materials selected by the invention is micron-sized, so that the grain diameter of the nylon powder selected by the invention is less than 5 mu m. The particle sizes of the nylon powder, the melt spinning additive and the auxiliary material are all in the micron order, so that high-temperature melt mixing is not needed, the three materials are directly mixed and tableted at the selected temperature range of 0-200 ℃ to prepare the blended spinning master batch, and the blended spinning master batch needs to be disintegrated in a molten nylon raw material to provide the melt spinning additive, so that the blended spinning master batch is easy to disintegrate, and needs to have certain hardness to facilitate packaging and transportation, therefore, the pressure range of pressure forming is selected to be 0.1-10 MPa, and the blended master batch raw material prepared in the step A is pressurized to prepare the blended spinning master batch.

firstly, the effective concentration of the melt spinning additive and the auxiliary material in the blended spinning master batch is obviously improved;

secondly, the types and the contents of various additives and auxiliary materials in the blended spinning master batch are easier to control, and all components are uniformly dispersed;

thirdly, the blended spinning master batch has uniform size, is convenient to package, and can realize accurate quantitative addition of the spinning master batch in the subsequent melt spinning process;

fourthly, a high-temperature melting process is not adopted in the preparation process of the blended spinning master batch, so that the thermal degradation of nylon is effectively avoided, and the quality of the spun nylon fiber is ensured;

fifthly, the preparation process of the blended spinning master batch does not need high-temperature operation, reduces energy consumption, is green and environment-friendly, reduces production cost, and simultaneously ensures that the production, processing and preparation processes are safer and more reliable.

Examples

Experimental part

1. The terms used are:

(1) all "parts" referred to in the examples are "parts by weight".

(2) Reference to "hardness" in the examples means: and testing by a flat plate upper and lower tabletting tester to obtain the ultimate pressure of the blended spinning master batch during crushing.

2. The used raw material sources are as follows:

(1) nylon 6 slicing: high speed spun pure nylon 6 chips from Ningbo Henrun corporation;

（2）LaCl₃(anhydrous lanthanum chloride): huizhou city Power technologies, Inc.;

（3）Y(NO₃)₃(anhydrous yttrium nitrate): zibo lanthanide series worker Co., Ltd;

（4）Ce₂(SO₄)₃(anhydrous cerium sulfate): zibo Rabokang rare earth materials Co., Ltd.

Example 1

Pulverizing nylon 6 slices together with a grinder to obtain nylon powder with diameter of 5 μm, and mixing the obtained nylon powder with melt spinning additive Y (NO)₃)₃Mixing (anhydrous yttrium nitrate) according to the weight ratio of 9:1 to prepare master batch, adding dispersant tristearin (HTG) and disintegrant dry starch into the master batch according to the weight ratio of 100:1 and 100:3 of the master batch to the auxiliary materials respectively, and preparing the blending master batch raw material.

Pressurizing the prepared blending master batch raw material by a manual tablet press, and forming under the pressure of 1MPa to obtain the tablet blending spinning master batch.

10 pieces of the blended spinning masterbatch prepared in this experimental example were taken for analysis and test, and the relevant experimental test data are shown in table 1 below.

TABLE 1

Example 2

Pulverizing nylon 6 slices together with a grinder to obtain nylon powder with diameter of 2 μm, and mixing the obtained nylon powder with melt spinning additive Y (NO)₃)₃Mixing (anhydrous yttrium nitrate) according to the weight ratio of 9:1 to prepare master batch, adding dispersant tristearin (HTG) into the master batch according to the weight ratio of 100:1 and 100:0.5 of the master batch to the auxiliary materials respectively, and dissolving the dispersant tristearin (HTG) into the master batchBorax is used as the raw material of the blending master batch.

And pressurizing the prepared blending master batch raw material by an automatic tablet press, and forming under the pressure of 1.2MPa to obtain the tablet blending spinning master batch.

10 pieces of the blended spinning masterbatch prepared in this experimental example were taken for analysis and test, and the relevant experimental test data are shown in table 2 below.

TABLE 2

Example 3

Crushing nylon 6 slices by a grinder to obtain nylon powder with the diameter of 1 mu m, and mixing the obtained nylon powder with a melt spinning additive Ce₂(SO₄)₃Mixing (anhydrous cerium sulfate) according to the weight ratio of 7:3 to prepare master batch, adding lubricant silicone oil and adhesive acrylic resin into the master batch according to the weight ratio of 100:2 and 100:0.5 of the master batch to the auxiliary materials respectively, and preparing the blending master batch raw material.

Pressurizing the prepared blending master batch raw material by a manual tablet press, and forming under the condition of 0.4MPa of pressure intensity to obtain the drug-flake blending spinning master batch.

10 pieces of the blended spinning masterbatch prepared in this experimental example were taken for analysis and test, and the relevant experimental test data are shown in table 3 below.

TABLE 3

Example 4

Crushing nylon 6 slices by a grinder to obtain nylon powder with the diameter of 0.5 mu m, and mixing the obtained nylon powder with a melt spinning additive Ce₂(SO₄)₃Mixing (anhydrous cerium sulfate) according to the weight ratio of 7:3 to prepare master batch, adding a lubricant graphite fluoride and a cosolvent sodium benzoate into the master batch according to the weight ratio of 100:3 and 100:1 of the master batch to the auxiliary materials respectively, and preparing the blending master batch raw material.

And pressurizing the prepared blending master batch raw material by an automatic tablet press, and forming under the condition that the pressure intensity is 0.5MPa to obtain the tablet blending spinning master batch.

10 pieces of the blended spinning masterbatch prepared in this experimental example were taken for analysis and test, and the relevant experimental test data are shown in table 4 below.

TABLE 4

Example 5

Pulverizing nylon 6 slice with a grinder to obtain nylon powder with diameter of 0.2 μm, and mixing the nylon powder with melt spinning additive LaCl₃Mixing (anhydrous lanthanum chloride) according to the weight ratio of 1:1 to prepare master batch, adding lubricant silicone oil and coating agent hydroxypropyl methylcellulose (HPMC) into the master batch according to the weight ratio of 100:5 and 100:0.5 of the master batch to the auxiliary materials respectively to prepare the blending master batch raw material.

Pressurizing the prepared blending master batch raw material by a manual tablet press, and forming under the condition of 0.3MPa of pressure intensity to obtain the drug-flake blending spinning master batch.

10 pieces of the blended spinning masterbatch prepared in this experimental example were taken for analysis and test, and the relevant experimental test data are shown in table 5 below.

TABLE 5

Example 6

Pulverizing nylon 6 slice with a grinder to obtain nylon powder with diameter of 0.1 μm, and mixing the nylon powder with melt spinning additive LaCl₃Mixing (anhydrous lanthanum chloride) according to the weight ratio of 1:1 to prepare master batch main material, adding lubricant silicone oil and coating agent hydroxypropyl cellulose (HPC) into the master batch main material according to the weight ratio of the master batch main material to the auxiliary material of 100:2 and 100:0.5 respectively to prepare the blending master batch raw material.

And pressurizing the prepared blending master batch raw material by an automatic tablet press, and forming under the condition that the pressure intensity is 0.4MPa to obtain the tablet blending spinning master batch.

10 pieces of the blended spinning masterbatch prepared in this experimental example were taken for analysis and test, and the relevant experimental test data are shown in table 6 below.

TABLE 6

Comparative example

Comparative example 1

Adding LaCl₃The (anhydrous lanthanum chloride) and the nylon 6 chips are produced into blended spinning master batches by a conventional melt blending method according to the following weight ratio.

3 of the blended spinning masterbatch prepared in each mass ratio were analyzed and tested, and the experimental data are shown in table 7 below.

TABLE 7

Examples of the experiments

The spinning masterbatch prepared in the above examples 1 to 6 and comparative example 1 was used for melt spinning, and the spinning process parameters are shown in the following table 8:

TABLE 8

The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.

Claims

1. The fine denier nylon raw material blending spinning master batch is characterized in that the blending spinning master batch comprises:

the nylon comprises: nylon 6, nylon 66, nylon 10, nylon 12, nylon 1212 and nylon 610;

the metal is selected from:

wherein,

2. The fine denier nylon raw material blending spinning masterbatch according to claim 1, wherein the weight ratio of the nylon powder to the melt spinning additive is 1: 3-3: 1.

3. The fine denier nylon raw material blended spinning masterbatch according to claim 1, wherein the weight ratio of the masterbatch main material to the auxiliary material is 10: 1-100: 2.

4. The fine denier nylon raw material blended spinning masterbatch of claim 1, wherein the dispersant is glyceryl tristearate.

5. The fine denier nylon raw material blended spinning masterbatch of claim 1, wherein the binder is acrylic resin.

6. The fine denier nylon raw material blended spinning masterbatch of claim 1, wherein the disintegrant is dry starch.

7. The fine denier nylon raw material blended spinning masterbatch of claim 1, wherein the cosolvent is selected from sodium benzoate or borax.

8. The fine denier nylon raw material blended spinning masterbatch of claim 1, wherein the lubricant is selected from silicone oil or graphite fluoride.

9. The fine denier nylon raw material blended spinning masterbatch of claim 1, wherein the coating agent is selected from hydroxypropyl methyl cellulose or hydroxypropyl cellulose, used alone or in combination.

10. The fine denier nylon raw material blended spinning masterbatch of claim 1, wherein the blended spinning masterbatch is prepared by the following steps: