Recycled Colored Bulk Continuous Filament Polyester Prepared by Hierarchical Shading and Color Mixing Technology

Abstract

The present invention relates to a recycled colored polyester bulked continuous filament prepared by a hierarchical shading color matching technology, belonging to the technical field of fiber materials. The present invention uses waste colored polyester, conventional semi-dull polyester, masterbatch, zinc acetate, antimony trioxide, and a self-made reinforcing agent as raw materials to prepare a polyester recycled material colored fiber based on the hierarchical shading color matching technology. The preparation method of the present invention classifies waste colored polyester by color system, uses a self-made reinforcing agent for chain extension, then adds a dark color masterbatch for color shading, and adds conventional polyester chips to mix and melt-spin to obtain a recycled colored polyester bulked continuous filament. The present invention uses the hierarchical shading color matching technology to directly produce recycled colored polyester bulked continuous filaments from waste colored polyester without decolorizing the colored waste polyester, which is green and environmentally friendly. The prepared recycled colored bulked continuous filaments have good strength and resilience and can be widely used in the field of carpet filaments.

Description

Technical Field

[0001] The present invention belongs to the technical field of fiber materials, and specifically relates to a recycled colored regenerated polyester bulked continuous filament prepared by a hierarchical shading and color mixing technology. Background Art

[0002] Due to its excellent physical and chemical properties, polyester fiber is widely used in the field of carpet yarns, which has also led to an increasing amount of waste polyester. Since polyester is difficult to biodegrade, its waste accumulates in large quantities and even flows into the ocean, causing serious environmental pollution. Carpet yarn is a kind of silk material used to make carpets, usually made of natural fibers or synthetic fibers. The production process of carpet yarn includes steps such as raw material preparation, melt spinning, and twisting and setting.

[0003] In the prior art, although colored polyester accounts for a large proportion in waste polyester, due to the high cost and great difficulty of decolorization and separation and purification, it is generally landfilled, incinerated, or downgraded and applied to products with low color requirements such as carpets, engineering fillers, and asphalt. Based on this, the present invention provides a recycled colored regenerated polyester bulked continuous filament prepared by a hierarchical shading and color mixing technology, which directly uses waste colored polyester to prepare recycled colored polyester bulked continuous filament (BCF) without decolorization treatment. Summary of the Invention

[0004] The purpose of the present invention is to provide a recycled colored regenerated polyester bulked continuous filament prepared by a hierarchical shading and color mixing technology to solve the problems mentioned in the above background art.

[0005] The purpose of the present invention can be achieved by the following technical solutions:

[0006] The recycled colored regenerated polyester bulked continuous filament prepared by the hierarchical shading and color mixing technology comprises the following raw materials: recycled colored polyester modified by a reinforcing agent, conventional semi-dull polyester, and dark masterbatch of the same color system, wherein the weight part formula is: recycled colored polyester modified by a reinforcing agent > 51 parts, conventional semi-dull polyester < 49 parts, and 1 - 10 parts of dark masterbatch of the same color system;

[0007] The preparation method of the recycled colored regenerated polyester bulked continuous filament comprises the following steps:

[0008] First step, classify waste colored polyester by color system to obtain recycled colored polyester;

[0009] Step 2: Put the classified recycled colored polyester, zinc acetate, and antimony trioxide into a reflux reaction vessel protected by nitrogen, add the self-made enhancer, evacuate the pressure in the reaction vessel to 0.01 - 0.05 KPa, and then carry out a polymerization reaction at 260 - 270 °C for 2 - 4 h to obtain the recycled colored polyester modified by the enhancer;

[0010] Step 3: Mix the recycled colored polyester modified by the enhancer, the conventional semi-dull polyester, and the dark masterbatch of the same color system, add them into a twin-screw extruder, melt and extrude, and then spin to obtain a recycled colored polyester drawn textured filament prepared based on the hierarchical shading color mixing technology.

[0011] Furthermore, the mass ratio of the classified recycled polyester, zinc acetate, antimony trioxide, and self-made enhancer used in Step 2 is 100:0.4:0.08 - 0.1:5.

[0012] Furthermore, the mass fraction ratio of the recycled colored polyester modified by the enhancer, the conventional semi-dull polyester, and the dark masterbatch of the same color system in Step 3 is 51 - 80:20 - 49:3 - 10.

[0013] Furthermore, the parameter settings of the twin-screw extruder in Step 3 are: Zone 1 at 290 °C, Zone 2 at 295 °C, Zone 3 at 295 °C, Zone 4 at 300 °C, Zone 5 at 295 °C, Zone 6 at 290 °C, and the screw speed is 50 rpm.

[0014] Furthermore, the enhancer is prepared by the following steps:

[0015] Step 1: Mix 4-methylaminobenzoic acid, epichlorohydrin, and N,N-dimethylformamide in a three-necked flask, install a condenser and a thermometer, start magnetic stirring, and react at 70 - 90 °C for 2 - 3 h. After the reaction is completed, rotary evaporate to remove the solvent, and then obtain Intermediate 1 through silica gel column chromatography;

[0016] Step 2: Mix Intermediate 1 and triethyl phosphite in a three-necked flask, install a condenser and a thermometer, start magnetic stirring, and react at 140 - 145 °C for 24 h. After the reaction is completed, rotary evaporate to remove triethyl phosphite to obtain Intermediate 2;

[0017] Step 3: Mix Intermediate 2, n-propyl bromide, and acetonitrile in a three-necked flask, install a condenser and a thermometer, start magnetic stirring, and react at 40 - 60 °C for 24 h. After the reaction is completed, rotary evaporate to remove the solvent, and then obtain the enhancer through silica gel column chromatography.

[0018] Further, the dosage ratio of 4-methylaminobenzoic acid, epichlorohydrin, and N,N-dimethylformamide used in Step 1 is 0.1 mol: 0.1 mol: 80 - 100 mL.

[0019] Further, the dosage ratio of Intermediate 1 and triethyl phosphite used in Step 2 is 0.08 mol: 0.12 - 0.15 mol.

[0020] Further, the dosage ratio of Intermediate 2, n-propyl bromide, and acetonitrile used in Step 3 is 0.04 mol: 0.04 - 0.06 mol: 40 - 60 mL.

[0021] Advantages of the present invention:

[0022] 1) The present invention uses recycled colored polyester, zinc acetate, antimony trioxide, and a self-made enhancer as raw materials to prepare polyester recycled colored fibers prepared by a hierarchical shading color mixing technology. The preparation method of the present invention classifies waste colored polyester by color system and then polymerizes and chain extends it with the self-made enhancer to obtain an enhancer-modified recycled colored polyester. Then, the enhancer-modified recycled colored polyester is mixed with conventional semi-dull polyester and dark color masterbatch and melt-spun to obtain polyester recycled colored fibers prepared by a hierarchical shading color mixing technology. The preparation method of the present invention uses a hierarchical shading color mixing technology to directly produce recycled colored polyester fibers from waste polyester without the need for decolorization treatment of waste colored polyester, which is green and environmentally friendly.

[0023] 2) The present invention uses 4-methylaminobenzoic acid and epichlorohydrin as raw materials. The imino group of 4-methylaminobenzoic acid and the epoxy group of epichlorohydrin undergo a nucleophilic addition reaction to obtain Intermediate 1. Then, using Intermediate 1 as a raw material, the chlorine atom of Intermediate 1 reacts with triethyl phosphite to undergo a Michaelis-Arbuzov reaction to obtain Intermediate 2. Finally, using Intermediate 2 as a raw material, the tertiary amine structure of Intermediate 2 reacts with n-propyl bromide to undergo a quaternary ammonium salt reaction to obtain an enhancer. The structure of the enhancer in the present invention contains hydroxyl and carboxyl groups, which can copolymerize with the products after the alcoholysis of waste polyester and combine in the colored polyester, thus taking effect stably for a long time. The phosphate ester structure in the enhancer of the present invention will form a dense protective carbon layer when reacting at high temperature, which can endow the colored polyester with good flame retardant effect. In addition, the enhancer of the present invention also has a quaternary ammonium salt structure, which can increase the charge density in the colored polyester and promote charge transfer after polymerization with the colored polyester, and can endow the colored polyester with good antistatic effect.

[0024] 3) The polyester recycled colored fibers prepared by the present invention based on the hierarchical shading color mixing technology are green and environmentally friendly and can be widely used in the field of carpet filaments. Specific embodiments

[0025] Next, in combination with the embodiments of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention.

[0026] Example 1

[0027] An enhancer is prepared by the following steps:

[0028] Step 1: Mix 0.1 mol of 4-methylaminobenzoic acid, 0.1 mol of epichlorohydrin, and 80 mL of N,N-dimethylformamide in a three-necked flask, install a condenser and a thermometer, turn on magnetic stirring, and react at 70 °C for 2 h. After the reaction is completed, rotary evaporate to remove the solvent, and then obtain Intermediate 1 through silica gel column chromatography;

[0029] Step 2: Mix 0.08 mol of Intermediate 1 and 0.12 mol of triethyl phosphite in a three-necked flask, install a condenser and a thermometer, turn on magnetic stirring, and react at 140 °C for 24 h. After the reaction is completed, rotary evaporate to remove triethyl phosphite to obtain Intermediate 2;

[0030] Step 3: Mix 0.04 mol of Intermediate 2, 0.04 mol of n-propyl bromide, and 40 mL of acetonitrile in a three-necked flask, install a condenser and a thermometer, turn on magnetic stirring, and react at 40 °C for 24 h. After the reaction is completed, rotary evaporate to remove the solvent, and then obtain the enhancer through silica gel column chromatography.

[0031] Example 2

[0032] An enhancer is prepared by the following steps:

[0033] Step 1: Mix 0.1 mol of 4-methylaminobenzoic acid, 0.1 mol of epichlorohydrin, and 90 mL of N,N-dimethylformamide in a three-necked flask, install a condenser and a thermometer, turn on magnetic stirring, and react at 80 °C for 2.5 h. After the reaction is completed, rotary evaporate to remove the solvent, and then obtain Intermediate 1 through silica gel column chromatography;

[0034] Step 2: Mix 0.08 mol of Intermediate 1 and 0.135 mol of triethyl phosphite in a three-necked flask, install a condenser and a thermometer, turn on magnetic stirring, and react at 142 °C for 24 h. After the reaction is completed, rotary evaporate to remove triethyl phosphite to obtain Intermediate 2;

[0035] Step 3: Mix 0.04 mol of intermediate 2, 0.05 mol of n-propyl bromide, and 50 mL of acetonitrile in a three-necked flask. Install a condenser and a thermometer, start magnetic stirring, and react at 50 °C for 24 h. After the reaction is completed, remove the solvent by rotary evaporation, and then obtain the enhancer through silica gel column chromatography.

[0036] Example 3

[0037] An enhancer is prepared by the following steps:

[0038] Step 1: Mix 0.1 mol of 4-methylaminobenzoic acid, 0.1 mol of epichlorohydrin, and 100 mL of N,N-dimethylformamide in a three-necked flask. Install a condenser and a thermometer, start magnetic stirring, and react at 90 °C for 3 h. After the reaction is completed, remove the solvent by rotary evaporation, and then obtain intermediate 1 through silica gel column chromatography.

[0039] Step 2: Mix 0.08 mol of intermediate 1 and 0.15 mol of triethyl phosphite in a three-necked flask. Install a condenser and a thermometer, start magnetic stirring, and react at 145 °C for 24 h. After the reaction is completed, remove triethyl phosphite by rotary evaporation to obtain intermediate 2.

[0040] Step 3: Mix 0.04 mol of intermediate 2, 0.06 mol of n-propyl bromide, and 60 mL of acetonitrile in a three-necked flask. Install a condenser and a thermometer, start magnetic stirring, and react at 60 °C for 24 h. After the reaction is completed, remove the solvent by rotary evaporation, and then obtain the enhancer through silica gel column chromatography.

[0041] Example 4

[0042] The polyester recycled colored fiber prepared by the hierarchical shading color mixing technology comprises the following raw materials: waste polyester, conventional semi-dull polyester, masterbatch, zinc acetate, antimony trioxide, and the enhancer obtained in Example 1;

[0043] The preparation method of the polyester recycled colored fiber comprises the following steps:

[0044] The first step: Classify the waste colored polyester by color system to obtain recycled colored polyester.

[0045] The second step: Put the classified recycled colored polyester, zinc acetate, and antimony trioxide into a reflux reaction vessel protected by nitrogen, add the self-made enhancer, and evacuate the pressure in the reaction vessel to 0.02 KPa, and then carry out a polymerization reaction at 260 °C for 2 h to obtain the recycled colored polyester modified with the enhancer; wherein, the mass ratio of the classified recycled polyester, zinc acetate, antimony trioxide, and self-made enhancer used in this example is 100:0.4:0.08:5.

[0046] Step 3: Mix the recycled colored polyester modified with the enhancer, the conventional semi-dull polyester, and the dark masterbatch of the same color system in a mass ratio of 75:20:5, then add them into a twin-screw extruder for melt extrusion and spinning to obtain a colored fiber of recycled polyester material prepared based on the hierarchical shading color mixing technology. Among them, in this embodiment, the parameter settings of the twin-screw extruder are: zone 1 at 290 °C, zone 2 at 295 °C, zone 3 at 295 °C, zone 4 at 300 °C, zone 5 at 295 °C, zone 6 at 290 °C, and the screw speed is 50 rpm;

[0047] After the colored fiber of recycled polyester material prepared by the hierarchical shading color mixing technology is melt-extruded, it is cooled slowly by side blowing, oiled, heat-drawn, thermally jet-deformed, and air-cooled, and then wound to obtain a colored fiber carpet yarn of recycled polyester material.

[0048] Example 5

[0049] The colored fiber of recycled polyester material prepared by the hierarchical shading color mixing technology contains the following raw materials: waste polyester, conventional semi-dull polyester, masterbatch, zinc acetate, antimony trioxide, and the enhancer obtained in Example 2;

[0050] The preparation method of the colored fiber of recycled polyester material includes the following steps:

[0051] Step 1: Classify the waste colored polyester by color system to obtain recycled colored polyester;

[0052] Step 2: Put the classified recycled colored polyester, zinc acetate, and antimony trioxide together into a reflux reaction vessel under nitrogen protection, add the self-made enhancer, and evacuate the pressure in the reaction vessel to 0.02 KPa, and then carry out a polymerization reaction at a temperature of 260 °C for 2 h to obtain the recycled colored polyester modified with the enhancer; among them, in this embodiment, the mass ratio of the classified recycled polyester, zinc acetate, antimony trioxide, and self-made enhancer used is 100:0.4:0.1:5.

[0053] Step 3: Mix the recycled colored polyester modified with the enhancer, the conventional semi-dull polyester, and the dark masterbatch of the same color system in a mass ratio of 60:35:5, then add them into a twin-screw extruder for melt extrusion and spinning to obtain a colored fiber of recycled polyester material prepared based on the hierarchical shading color mixing technology. Among them, in this embodiment, the parameter settings of the twin-screw extruder are: zone 1 at 290 °C, zone 2 at 295 °C, zone 3 at 295 °C, zone 4 at 300 °C, zone 5 at 295 °C, zone 6 at 290 °C, and the screw speed is 50 rpm;

[0054] After the polyester recycled colored fiber prepared by the graded shading color mixing technology is melt-extruded, it is cooled slowly by side blowing, oiled, heat-drawn, thermally jet-deformed and air-cooled, and then wound to obtain polyester recycled colored fiber carpet yarns.

[0055] Example 6

[0056] The polyester recycled colored fiber prepared by the graded shading color mixing technology contains the following raw materials: waste polyester, conventional semi-dull polyester, masterbatch, zinc acetate, antimony trioxide, and the reinforcing agent obtained in Example 3;

[0057] The preparation method of the polyester recycled colored fiber includes the following steps:

[0058] First step, classify the waste colored polyester by color system to obtain recycled colored polyester;

[0059] Second step, put the classified recycled colored polyester, zinc acetate, and antimony trioxide into a reflux reaction vessel protected by nitrogen, add the self-made reinforcing agent, and evacuate the pressure in the reaction vessel to 0.02 KPa, and then carry out a polymerization reaction at 260 °C for 2 h to obtain recycled colored polyester modified with the reinforcing agent; among them, the mass ratio of the classified recycled polyester, zinc acetate, antimony trioxide, and self-made reinforcing agent used in this example is 100:0.4:0.09:5.

[0060] Third step, mix the recycled colored polyester modified with the reinforcing agent, conventional semi-dull polyester, and dark masterbatch of the same color system in a mass ratio of 55:40:5, add them to a twin-screw extruder, melt-extrude and then spin to obtain a polyester recycled colored fiber prepared based on the graded shading color mixing technology. Among them, the parameter settings of the twin-screw extruder in this example are: zone 1 at 290 °C, zone 2 at 295 °C, zone 3 at 295 °C, zone 4 at 300 °C, zone 5 at 295 °C, zone 6 at 290 °C, and the screw speed is 50 rpm;

[0061] After the polyester recycled colored fiber prepared by the graded shading color mixing technology is melt-extruded, it is cooled slowly by side blowing, oiled, heat-drawn, thermally jet-deformed and air-cooled, and then wound to obtain polyester recycled colored fiber carpet yarns.

[0062] Comparative Example 1

[0063] A polyester recycled colored fiber prepared based on the graded shading color mixing technology contains the following raw materials: waste polyester, conventional semi-dull polyester, masterbatch, zinc acetate, antimony trioxide;

[0064] The preparation method of the polyester recycled colored fiber includes the following steps:

[0065] Step 1: Classify waste polyester by color system to obtain recycled colored polyester for recycling.

[0066] Step 2: Put the classified recycled colored polyester, zinc acetate, and antimony trioxide into a reflux reaction vessel protected by nitrogen, evacuate the pressure in the reaction vessel to 0.04 KPa, and then carry out a polymerization reaction at 270 °C for 2 h to obtain recycled colored polyester modified with an enhancer. Among them, the mass ratio of the classified recycled polyester, zinc acetate, and antimony trioxide used in this example is 100:0.4:0.09.

[0067] Step 3: Mix recycled colored polyester, conventional semi-dull polyester, and dark masterbatch of the same color system in a mass ratio of 80:10:10, add them into a twin-screw extruder, melt and extrude, and then spin to obtain a polyester recycled colored fiber prepared based on the hierarchical shading color mixing technology. Among them, the parameter settings of the twin-screw extruder in this example are: zone 1 at 290 °C, zone 2 at 295 °C, zone 3 at 295 °C, zone 4 at 300 °C, zone 5 at 295 °C, zone 6 at 290 °C, and the screw speed is 50 rpm.

[0068] Comparative Example 2

[0069] This comparative example is a commercially available environmentally friendly recycled DTY polyester.

[0070] The recycled colored polyester drawn textured yarns prepared by the hierarchical shading color mixing technology in Examples 4-6 and Comparative Example 1 and the commercially available environmentally friendly recycled polyester drawn textured yarn in Comparative Example 2 were tested for breaking strength using the national standard GB / T14344-2022 "Test Method for Tensile Properties of Chemical Fibre Filaments", and the thermal shrinkage rate was tested with reference to the national standard GB / T6505-2017 "Test Method for Thermal Shrinkage Rate of Chemical Fibre Filaments (After Treatment)". The test results are shown in Table 1:

[0071] Table 1

[0072] Project Breaking strength (cN / dtex) Heat shrinkage rate (%) Example 4 5.7 10 Example 5 4.5 12 Example 6 3.8 14 Comparative Example 1 2.7 17 Comparative Example 2 2.4 18

[0073] As can be seen from Table 1, for a kind of recycled colored polyester bulked continuous filament prepared by the hierarchical shading color mixing technology in Examples 4-6 of the present invention, its breaking strength is higher than that of the commercially available recycled polyester bulked continuous filament, and its thermal shrinkage rate is lower than that of the commercially available recycled polyester bulked continuous filament, indicating that the polyester recycled material colored fiber prepared by the hierarchical shading color mixing technology of the present invention has good mechanical properties. Comparative Example 1 carried out a control experiment on the reinforcing agent used in the present invention. Without using the reinforcing agent of the present invention, the obtained recycled colored polyester bulked continuous filament has a low breaking strength and a high thermal shrinkage rate. This shows the effectiveness of the reinforcing agent of the present invention. In summary, the preparation method of the present invention is green and environment-friendly, and the prepared recycled colored polyester bulked continuous filament has good properties and can be widely used in the field of carpet filaments.

[0074] The above has introduced in detail a kind of polyester recycled material colored fiber prepared by the hierarchical shading color mixing technology provided by the present invention. Specific examples are used in this article to elaborate on the principle and implementation manner of the present invention. The description of the above embodiments is only used to help understand the method and its core idea of the present invention, including the best mode, and also enables any person skilled in the art to practice the present invention, including manufacturing and using any device or system, and implementing any combination method. It should be noted that for those of ordinary skill in the art in this technical field, without departing from the principle of the present invention, several improvements and modifications can be made to the present invention. In particular, as long as there is no structural conflict, the various features in the embodiments disclosed by the present invention can be combined with each other in any way, and the exhaustive description of these combinations is not given in this specification only for the sake of saving space and resources. Therefore, the present invention is not limited to the specific embodiments disclosed in the text, but includes all technical solutions falling within the scope of the claims.

Claims

1. Recycled colored polyester bulked filament prepared by graded color shading technology, characterized in that: The raw materials include: recycled colored polyester modified by reinforcing agent, conventional semi-matt polyester, dark masterbatch of the same color series; Wherein, the reinforcing agent is prepared by the following steps: Step 1, 4-methylaminobenzoic acid, epichlorohydrin and N,N-dimethylformamide are mixed in a container, stirred evenly, and reacted at a temperature of 70-90° C. for 2-3 hours to obtain intermediate 1; Step 2, intermediate 1 and triethyl phosphite are mixed in a container, stirred evenly, and reacted at a temperature of 140-145° C. for 24 hours to obtain intermediate 2; Step 3, the intermediate 2, n-propyl bromide and acetonitrile are mixed in a container, stirred evenly, and reacted at a temperature of 40-60° C. for 24 hours to obtain the enhancer; The reinforcing agent-modified recycled colored polyester is obtained by subjecting the recycled colored polyester to polymerization and chain extension modification with a reinforcing agent.

2. The recycled colored polyester bulked filament prepared by the graded color-shading coloring technology according to claim 1, characterized in that: The amount ratio of 4-methylaminobenzoic acid, epichlorohydrin and N,N-dimethylformamide used in step 1 is 0.1 mol: 0.1 mol: 80-100 mL.

3. The recycled colored polyester bulked filament prepared by the graded color-shading coloring technology according to claim 1, characterized in that: The usage ratio of intermediate 1 and triethyl phosphite used in step 2 is 0.08 mol: 0.12-0.15 mol.

4. The recycled colored polyester bulked filament prepared by the graded color-shading coloring technology according to claim 1, characterized in that: The amount ratio of intermediate 2, n-propyl bromide and acetonitrile used in step 3 is 0.04 mol: 0.04-0.06 mol: 40-60 mL.

5. The recycled colored polyester bulked filament prepared by the graded color-shading coloring technology according to claim 1, characterized in that: The method for preparing the polyester recycled colored fiber comprises the following steps: The first step is to classify the waste colored polyester according to the color system to obtain the recycled colored polyester; The second step is to put the classified recycled colored polyester, zinc acetate and antimony trioxide into a nitrogen-protected reflux reaction vessel, add a homemade enhancer, and pump the pressure in the reaction vessel to 0.01-0.05 KPa, and then perform a polymerization reaction at a temperature of 260-270° C. for 2-4 hours to obtain a recycled colored polyester modified with an enhancer; In the third step, the reinforcing agent-modified recycled colored polyester, conventional semi-dull polyester and dark masterbatch of the same color system are mixed and added into a twin-screw extruder for melt extrusion and then spun to obtain a recycled colored polyester bulked filament prepared by a graded color shading technology.

6. The recycled colored polyester bulked filament prepared by the graded color-shading coloring technology according to claim 5, characterized in that: The mass ratio of the classified recycled polyester, zinc acetate, antimony trioxide and homemade reinforcing agent used in the second step is 100:0.4:0.08-0.1:

5.

7. The recycled colored polyester bulked filament prepared by the graded color-shading coloring technology according to claim 5, characterized in that: The mass fraction ratio of the reinforcing agent-modified recycled colored polyester, conventional semi-dull polyester and dark masterbatch of the same color system in the third step is 51-80:20-49:3-10.

8. The recycled colored polyester bulked filament prepared by the graded color-shading coloring technology according to claim 5, characterized in that: In the third step, the parameters of the twin-screw extruder were set as 290°C in zone 1, 295°C in zone 2, 295°C in zone 3, 300°C in zone 4, 295°C in zone 5, 290°C in zone 6, and a screw speed of 50 rpm.