CN105648572A - Black fine denier industrial polyester special filament and preparation method thereof - Google Patents

Abstract

The invention provides a special polyester filament for black fine denier industry and a preparation method thereof, wherein the preparation method comprises the following steps: the super-bright polyester color master batch comprises super-bright polyester and black color master batch, wherein the black color master batch comprises the following materials in percentage by weight: 30-50% of polyethylene terephthalate, 30-50% of polybutylene terephthalate, 10-30% of carbon black and 0.4-12% of auxiliary additives. The preparation method provided by the invention has the advantages that the polyester chips with common viscosity are adopted, the melt spinning method is utilized, the production cost is greatly saved from the raw material cost, the process flow is short, the energy consumption is low, the head interruption rate in the production process is low, and the produced filaments can meet the requirements of medium-high-strength sewing threads; and the method adopts a mode of directly adding carbon black to replace a mode of spinning and dyeing to prepare the black FDY polyester filament sewing thread, thereby avoiding the phenomena of environmental pollution, bleaching and decoloring, light intolerance, unstable chemical property and the like caused by black dye dyeing.

Description

Black fine denier industrial polyester special filament and preparation method thereof

technical field

The invention relates to the field of chemical fibers, in particular to a black fine denier industrial polyester special filament and a preparation method thereof.

Background technique

Polyester sewing thread includes polyester filament sewing thread and polyester short thread sewing thread, and polyester filament sewing thread has the advantages of high strength, soft thread quality, no mildew, good seamability, stable physical and chemical properties and no joints, etc., and is widely used Used in high-end clothing, bags, shoes and hats, military supplies and other fields.

The technology of polyester filament for sewing thread at home and abroad mainly includes spinning and pulling one-step method (FDY method (FULLDRAWYARN)), UDY-DT two-step method and POY-DT (PARTIALLYORIENTEDYARN) two-step method. The FDY method uses high-viscosity polyester chips, and a slow cooling device needs to be added to the spinning process, and the manufacturing cost is high, especially when producing fine denier yarns below 150D. The UDY-DT two-step method first spins undrawn yarn, and then performs multi-stage high-stretching, but the strength of the obtained polyester filament is not high, lacks effective setting, and has a high thermal shrinkage rate, which has been basically eliminated. Chinese patent CN200610085250 adopts the POY-DT two-step method to produce fine denier high-strength low-shrinkage and low-elongation polyester filaments through the steps of primary stretching, tension heat setting, secondary stretching, relaxation heat setting and winding. The obtained polyester filament strength and boiling water shrinkage can meet the requirements of medium and high-grade filament sewing threads. However, its process flow is long, energy consumption is high, and the end-stop rate in the production process is high, resulting in high production costs.

At present, few manufacturers use the method of adding color masterbatch to prepare black medium and high-strength polyester filaments. The reason is that inorganic carbon black particles are non-melting, and they are unevenly distributed in the fiber during high-strength drafting, which is easy to form agglomeration. With the increase of draft ratio, the rate of end breakage increases more significantly, so that the black high-strength silk is still prepared by dyeing.

Contents of the invention

A brief overview of the invention is given below in order to provide a basic understanding of some aspects of the invention. It should be understood that this summary is not an exhaustive overview of the invention. It is not intended to identify key or critical parts of the invention nor to delineate the scope of the invention. Its purpose is merely to present some concepts in a simplified form as a prelude to the more detailed description that is discussed later.

The purpose of the present invention is to provide a kind of medium high strength, low thermal shrinkage rate black fine denier industrial polyester special filament and its preparation method, to solve the problems in the production process of medium high strength, low thermal shrinkage fine denier industrial polyester special filament in the background technology. High consumption, long technological process, and high cost; and solve the technical problem that the preparation of black medium and high-strength silk still adopts the dyeing method.

The invention provides a kind of black fine denier industrial polyester special filament, comprising: super glossy polyester and black color masterbatch, wherein the mass fraction of the black color masterbatch in the super glossy polyester is 3-4 %, the black color masterbatch includes the following materials: 30-50% polyethylene terephthalate, 30-50% polybutylene terephthalate, 10-30% carbon Black and 0.4-12% of auxiliary additives.

The present invention also provides a method for preparing black fine denier industrial polyester special filament, comprising the steps of:

S101: drying the super-bright polyester chips and the black masterbatch, so as to increase the viscosity and homogenize the viscosity of the super-bright polyester chips;

S102: mixing the super-bright polyester chips and the black masterbatch through a screw extruder for melt extrusion;

S103: Filter the extruded melt through a filter to remove impurities in the melt, and then mix it uniformly with a static mixer;

S104: The mixed melt is spun through the spinning box, and then the filament is cooled and oiled by the oil tanker. The oiled filament passes through the guide rod to increase the spinning tension, and then passes through the pre-netting device. oil homogenization;

S105: The filament after the pre-netting device enters the drafting device for drafting and heat setting, the drawn filament is networked by the main networker, and the networked tow is then processed by the winding head winding.

The black fine-denier industrial polyester special filament and its preparation method provided by the present invention utilize the melt-spinning method by adopting polyester chips (0.64-0.68dL/g) of ordinary viscosity, first greatly saving the production cost from the raw material cost, Secondly, the production method of the present invention has a short process flow, low energy consumption, and a low end-break rate in the production process, and the produced filaments can meet the requirements of medium and high-strength sewing threads; and the present invention uses the method of directly adding carbon black to replace The black FDY polyester filament sewing thread is prepared by spinning first and then dyed to avoid environmental pollution, rinsing and decolorization, light resistance, and chemical instability caused by black dyeing.

Description of drawings

In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only These are some embodiments of the present invention. Those skilled in the art can also obtain other drawings based on these drawings without creative work.

Fig. 1 is the flow chart of the method for preparing black fine denier industrial polyester special filament in the present invention.

detailed description

In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments It is a part of embodiments of the present invention, but not all embodiments. Elements and features described in one drawing or one embodiment of the present invention may be combined with elements and features shown in one or more other drawings or embodiments. It should be noted that representation and description of components and processes that are not related to the present invention and known to those of ordinary skill in the art are omitted from the drawings and descriptions for the purpose of clarity. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.

Embodiment one:

The invention provides a kind of black fine denier industrial polyester special filament, comprising: super glossy polyester and black color masterbatch, wherein the mass fraction of the black color masterbatch in the super glossy polyester is 3-4 %, the black color masterbatch includes the following materials: 30-50% polyethylene terephthalate, 30-50% polybutylene terephthalate, 10-30% carbon Black and 0.4-12% of auxiliary additives.

Optionally, the auxiliary additives include: 0.1-3% heat stabilizer, 0.1-3% antioxidant, 0.1-5% dispersant, and 0.1-1% coupling agent.

Optionally, the heat stabilizer is one or more of the following: stearates, organotin mercaptans, and dibutyltin laurate.

Optionally, the antioxidant is one or more of the following: 1010, 1330, 168, MARK5118A.

Optionally, the dispersant is one or more of the following: polyethylene wax, CH series; the coupling agent is titanate.

In the present invention, by adopting polyester chips with ordinary viscosity and using the melting spinning method, firstly, the production cost is greatly saved from the cost of raw materials, the broken end rate is low, and the produced filament can meet the requirements of medium and high-strength sewing threads; and In the present invention, the black FDY polyester filament sewing thread is prepared by directly adding carbon black instead of spinning first and then dyeing, so as to avoid environmental pollution, rinsing and decolorization, light resistance, unstable chemical properties and the like caused by black dyeing.

Embodiment two:

As shown in Figure 1, the present invention also provides a kind of black fine denier industrial polyester special filament preparation method, comprising steps:

S101: drying the super-bright polyester chips and the black masterbatch, so as to increase the viscosity and homogenize the viscosity of the super-bright polyester chips;

S102: mixing the super-bright polyester chips and the black masterbatch through a screw extruder for melt extrusion;

S103: Filter the extruded melt through a filter to remove impurities in the melt, and then mix it uniformly with a static mixer;

S104: The mixed melt is spun through the spinning box, and then the filament is cooled and oiled by the oil tanker. The oiled filament passes through the guide rod to increase the spinning tension, and then passes through the pre-netting device oil homogenization;

S105: The filament after the pre-netting device enters the drafting device for drafting and heat setting, the drawn filament is networked by the main networker, and the networked tow is then processed by the winding head winding.

The production method provided by the invention has short process flow, low energy consumption, low end-break rate in the production process, and the produced filaments can meet the requirements of medium and high-strength sewing threads.

Optionally, the ultra-bright polyester chips described in step S101 are dried through the combined use of a fluidized bed pre-crystallizer and a main drying tower, and the black color masterbatch is dried through a vacuum drum. The ultra-bright polyester chips are dried and thickened so that the moisture content of the super-bright polyester dry chips is ≤20ppm, which facilitates the implementation of the subsequent melt extrusion process, and makes the prepared parameters such as breaking strength and elongation comply with Require.

Optionally, the residence time of the super-bright polyester chips in the pre-crystallizer is 15-20min, and the pre-crystallization temperature is 175-185°C; the residence time of the super-bright polyester chips in the main drying tower It is 5.5-6.5h, and the main drying temperature is 168-172°C.

Optionally, the drafting device includes three hot rollers, the speed of the first hot roller is 550-750m/s, and the temperature is 105-115°C; the speed of the second hot roller is 2300-2400m/s , the temperature is 120-125°C; the speed of the third hot roller is 3200-3400m/s, and the heat setting temperature is 235-245°C. In the present invention, two drafts are carried out by three hot rollers, and the elongation at break of the filament is guaranteed while saving energy; wherein the first draft is carried out by the first hot roller and the second hot roller, and the second hot roller and the second hot roller The third hot roller performs the second drawing, and the third hot roller also has the function of heat setting, and the way of heat setting is tension heat setting.

Optionally, the winding speed is 3300-3450m/s.

In the preparation method of black fine denier industrial polyester special filament in the present invention, the production cost is largely saved at first from the cost of raw materials; secondly, the production method process flow in the present invention is shorter, the energy consumption is low, and the end-break rate in the production process is relatively low. Low, the filaments produced can meet the requirements of medium and high strength sewing threads.

Embodiment three:

Wet polyester chips are removed by vibrating sieves to remove powder and large particles, and then transported to the fluidized bed pre-crystallizer by a pulse device, staying in the pre-crystallizer for 15-20min, drying temperature 185°C, staying in the main drying tower for 6h, drying temperature 168°C, so that the moisture content of the slices after drying is ≤20ppm; and then distributed to each dry slice storage tank for later use.

It chooses A color masterbatch and dry super-bright polyester chips to be fed into a single-screw extruder at the same time for melt extrusion, wherein the characteristics of A color masterbatch are: the high-viscosity polyester chips (1.05- 1.15dL/g) content is 36.50%, polybutylene terephthalate content is 36.1%, carbon black content is 23%, heat stabilizer 0.15%, antioxidant 0.15%, dispersant 4.0%, coupling agent 0.1%; the addition ratio of color masterbatch and super bright polyester chips is 100:3.5.

Select A color masterbatch and use the metering valve to measure and feed the dry super-bright polyester chips into the single-screw extruder at the same time for melt extrusion. The screw is divided into six heating zones, and the temperature distribution of each zone is: Zone 1: 263-268°C, zone 2: 268-272°C, zone 3: 270-275°C, zone 4: 275-283°C, zone 5: 275-283°C, zone 6: 282-285°C, head temperature: 282 -285℃, head pressure: 13.5-15MPa.

Specifically, the temperature of each zone of the screw is set as: zone 1 266°C, zone 2 270°C, zone 3 275°C, zone 4 282, zone 5 282°C, zone 6 283°C, head temperature 285°C, pressure 15.0MPa.

The melt enters the melt filter after passing through the screw extruder, passes through the static mixer after coming out of the melt filter, and then enters the spinning box, wherein the outlet pressure of the pre-filter is 11.5Mpa, and is distributed to each metering Pump, the metering pump enters the spinning assembly after metering. The sand cup in the assembly is covered with a layer of non-woven fabric on its upper layer to increase pressure and filter performance, filter out agglomerates and large particles of carbon black, reduce end breakage rate, and increase spinnability.

After the tow is sprayed from the spinning assembly, it enters the side blowing cooling, wherein the side blowing wind speed is 0.4-0.6m/s, and the temperature is 22°C; then the filaments are oiled by the tanker, and the oiling rate is 0.8-1.5%. With the addition of carbon black, the surface roughness of the fiber becomes larger, and less oiling will easily cause the strength of the oil film on the surface of the filament to be low, resulting in an increase in end breaks. Therefore, the rate of end breaks can be reduced by increasing the oiling amount.

Take the specifications of spinning filaments as 150D/48f or 75D/24f or 100D/36f or 210D/48f as an example, set the side blowing wind speed to 0.45m/s, the temperature to 22°C, and the humidity to be 70%. The primary fiber is oiled by oil tanker, and the amount of oil is set at 1.2%; then pre-internetting is carried out to make the oil agent more uniform on the surface of the thread, and the pre-internetting pressure is set at 0.135MPa, which is slightly higher than that of ordinary white Large, to improve the twist force and the uniformity of the oil agent on the surface of the thread. After the thread is pre-networked, it enters the drafting hot roll and passes through the multi-stage hot roll for drafting and tension heat setting.

The present invention adopts the method of low-speed spinning and high-strength drafting, setting the speed of the first hot roller at 553m/s, the temperature at 110°C, and winding 8 turns; the speed of the second hot roller is 2320m/s, the temperature at 120°C, winding 5 turns , the speed of the third hot roller is 3273m/s, the temperature is 240°C, and the winding is 8 turns. The filament is tensioned and heat-set by the third hot roller and then enters the main network device for twisting to improve the cohesion and strength of the filament. The main network pressure: 0.3MPa; after passing through the main network, the filament enters the winding mechanism, setting The winding speed was 3230m/s. The physical properties of the prepared filaments are listed in Table 1.

The filament physical property prepared in the embodiment three of table 1

Embodiment four:

The polyester chips are passed through a vibrating screen to remove powder and large particles, and are transported to the fluidized bed pre-crystallizer by a pulse device, and stay in the pre-crystallizer for 15-20min at a drying temperature of 185°C, and stay in the main drying tower for 6h at a drying temperature of 168°C ℃, so that the water content of the slices after drying is ≤20ppm; and then distributed to each dry slice storage tank for later use.

It chooses B color masterbatch and dry super-bright polyester chips to be fed into a single-screw extruder at the same time for melt extrusion, wherein the characteristics of B color masterbatch are: the high-viscosity polyester chips (1.05- 1.15dL/g) content is 32.65%, polybutylene terephthalate content is 35%, carbon black content is 29%, heat stabilizer 0.1%, antioxidant 0.1%, dispersant 3%, coupling agent 0.15%. The ratio of color masterbatch to super bright polyester chips is 100:3.5.

Select B color masterbatch and use the metering valve to measure and feed the dry super-bright polyester chips into the single-screw extruder at the same time for melt extrusion. The third zone is 275°C, the fourth zone is 282°C, the fifth zone is 282°C, the sixth zone is 285°C, the head temperature is 285°C, and the pressure is 15MPa.

The melt enters the melt filter after passing through the screw extruder, passes through the static mixer after coming out of the melt filter, and then enters the spinning box, wherein the outlet pressure of the pre-filter is 11.5Mpa, and is distributed to each metering Pump, the metering pump enters the spinning assembly after metering. After the tow is ejected from the spinning assembly, it enters the side blowing cooling, wherein the wind speed of the side blowing is 0.4-0.6m/s; then the filament is oiled on the tanker, and the oiling rate is 0.8-1.5%. Due to the addition of carbon black, The roughness of the fiber surface becomes larger, and less oiling will easily cause the strength of the oil film on the surface of the filament to be low, resulting in an increase in end breakage. Therefore, the rate of end breakage can be reduced by increasing the oiling amount.

Take the specifications of spinning filaments as 150D/48f or 75D/24f or 100D/36f or 210D/48f as an example, set the side blowing wind speed to 0.45m/s, the temperature to 22°C, and the humidity to be 70%. The primary fiber is oiled by tanker, the amount of oil is set at 1.1%, and then the pre-network is carried out to make the oil agent more uniform on the surface of the thread, and the pre-network pressure is set at 0.135MPa, which is slightly higher than that of ordinary white. Large, to improve the twist force and the uniformity of the oil agent on the surface of the thread. After the thread is pre-networked, it enters the drafting hot roll and passes through the multi-stage hot roll for drafting and tension heat setting.

The present invention adopts the method of low-speed spinning and high-strength drafting, setting the speed of the first hot roller at 553m/s, the temperature at 110°C, and winding 8 turns; the speed of the second hot roller is 2320m/s, the temperature at 120°C, winding 5 turns , the speed of the third hot roller is 3269m/s, the temperature is 240°C, and the winding is 8 turns. After the filament is shaped by the third hot roller, it enters the main netting device for twisting to improve the cohesion and strength of the filaments. The main netting pressure: 0.3MPa; after passing through the main netting, the filaments enter the winding mechanism to set the winding The speed is 3230m/s. The physical properties of the prepared filaments are listed in Table 2.

The filament physical property prepared in the embodiment four of table 2

It can be seen from the above examples that the physical properties of silk are directly related to the drawing process and the masterbatch formula, and the difference is mainly reflected in the spinnability. This is because, on the one hand, the addition of antioxidants, thermal stabilizers and dispersants in masterbatch A is slightly larger than that of masterbatch B, which can effectively reduce the thermal degradation of the masterbatch; on the other hand, due to the carbon in masterbatch B The carbon black content in the masterbatch A is high, the carbon black aggregation is serious during spinning, the dispersibility is poor, and it is easy to cause broken ends during high-strength drafting. When the primary fiber is under a large post-drawing ratio, the strength of the yarn is ≥6.5cN/dtex, the shrinkage in boiling water is ≤4.0%, and the elongation at break is 15.0%±2%, which can meet the requirements of high-grade polyester filament sewing thread .

The preparation method in the present invention utilizes the method of melt-spinning by adopting the polyester chips of common viscosity, firstly greatly saved production cost from raw material cost, secondly the production method technological process among the present invention is shorter, and energy consumption is low, in production The end-stop rate in the process is low, and the produced filaments can meet the requirements of medium and high-strength sewing threads; and the present invention uses the method of directly adding carbon black to replace the method of first spinning and then dyeing to prepare black FDY polyester filament sewing threads to avoid black Environmental pollution, rinsing and decolorization, light resistance, chemical instability and other phenomena caused by dyeing.

In the above-mentioned embodiments of the present invention, the serial numbers and/or sequences of the embodiments are only for convenience of description, and do not represent the advantages and disadvantages of the embodiments. The description of each embodiment has its own emphases, and for the part that is not described in detail in a certain embodiment, refer to the relevant descriptions of other embodiments.

Finally, it should be noted that although the present invention and its advantages have been described in detail above, it should be understood that various changes, substitutions and modifications can be made without departing from the spirit and scope of the present invention defined by the appended claims. transform. Moreover, the scope of the present invention is not limited to the specific embodiments of the procedures, devices, means, methods and steps described in the specification. Those of ordinary skill in the art will readily appreciate from the disclosure of the present invention that existing and future designs that perform substantially the same function or obtain substantially the same results as the corresponding embodiments described herein can be used in accordance with the present invention. The developed process, device, means, method or steps. Accordingly, the appended claims are intended to include within their scope such processes, means, means, methods or steps.

Claims (10)

1. the black fine-denier special long filament of industry terylene, it is characterized in that, including: super glossy polyester and black Masterbatch, it is 3-4% that wherein said black Masterbatch accounts for the mass fraction of described super glossy polyester, and described black Masterbatch includes the material of following content: the auxiliary additive of the polyethylene terephthalate of 30-50%, the polybutylene terephthalate (PBT) of 30-50%, the white carbon black of 10-30% and 0.4-12%.

2. the black fine-denier special long filament of industry terylene according to claim 1, it is characterised in that described auxiliary additive includes: heat stabilizer 0.1-3%, antioxidant 0.1-3%, dispersant 0.1-5%, coupling agent 0.1-1%.

3. the black fine-denier special long filament of industry terylene according to claim 2, it is characterised in that described heat stabilizer is following one or more: stearates, organotin mercaptide compound, dibutyl tin laurate.

4. the black fine-denier special long filament of industry terylene according to claim 2, it is characterised in that described antioxidant is following one or more: 1010,1330,168, MARK5118A.

5. the black fine-denier special long filament of industry terylene according to claim 2, it is characterised in that described dispersant is following one or more: Tissuemat E, CH series; Described coupling agent is titanate ester.

6. the black fine-denier special filament preparation process of industry terylene as described in claim 1-5, it is characterised in that include step:

S101: super bright PET chips and black Masterbatch are dried, to carry out thickening and viscosity homogenizing to described super bright PET chips;

S102: described super bright PET chips is mixed with described black Masterbatch and is melt extruded by screw extruder;

S103: be filtered by filter by the melt of extrusion, removes the impurity in melt, subsequently by static mixer mix homogeneously;

S104: mixed melt carries out spinning through spinning manifold, is cooled down long filament subsequently and is oiled by oil tanker, and the long filament after oiling to increase spinning tension, then makes oil preparation homogenizing through pre-Network device by seal wire rod;

S105: the long filament after pre-Network device enters drafting system and carries out drawing-off and thermal finalization, and strand is carried out networking by master network device by the long filament after drawing-off, and the tow after networking is wound then through winding head.

7. the black fine-denier special filament preparation process of industry terylene according to claim 6, it is characterized in that, super bright PET chips described in shown step S101 is used in combination is dried by fluid bed pre-crystallizer and main drying tower, and described black Masterbatch is dried by vacuum drum.

8. the black fine-denier special filament preparation process of industry terylene according to claim 7, it is characterised in that described super bright PET chips time of staying in described pre-crystallizer is 15-20min, and pre-crystallization temperature is 175-185 DEG C;Described super bright PET chips time of staying in main drying tower is 5.5-6.5h, and main baking temperature is 168-172 DEG C.

9. the black fine-denier special filament preparation process of industry terylene according to claim 6, it is characterised in that

Described drafting system includes three hot-rollings, and described first hot-rolling speed is 550-750m/s, and temperature is 105-115 DEG C; Described second hot-rolling speed is 2300-2400m/s, and temperature is 120-125 DEG C; Described 3rd hot-rolling speed is 3200-3400m/s, and heat setting temperature is 235-245 DEG C.

10. the black fine-denier special filament preparation process of industry terylene according to claim 6, it is characterised in that described winding speed is 3300-3450m/s.