CN116656121A - Preparation method of color PA6 - Google Patents
Preparation method of color PA6 Download PDFInfo
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- CN116656121A CN116656121A CN202310530825.3A CN202310530825A CN116656121A CN 116656121 A CN116656121 A CN 116656121A CN 202310530825 A CN202310530825 A CN 202310530825A CN 116656121 A CN116656121 A CN 116656121A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 87
- 239000000049 pigment Substances 0.000 claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 24
- 239000000725 suspension Substances 0.000 claims abstract description 17
- 238000004043 dyeing Methods 0.000 claims description 17
- 238000001125 extrusion Methods 0.000 claims description 15
- 238000004108 freeze drying Methods 0.000 claims description 14
- 108091006172 SLC21 Proteins 0.000 claims description 8
- 102100032846 Solute carrier organic anion transporter family member 1A2 Human genes 0.000 claims description 8
- 239000003086 colorant Substances 0.000 claims description 8
- JBPWDTQELHPIPV-UHFFFAOYSA-N n-(3,6-dihydro-2h-pyridin-1-yl)pyridine-4-carboxamide Chemical compound C=1C=NC=CC=1C(=O)NN1CCC=CC1 JBPWDTQELHPIPV-UHFFFAOYSA-N 0.000 claims description 8
- 229920001469 poly(aryloxy)thionylphosphazene Polymers 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 230000004580 weight loss Effects 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 1
- 238000010907 mechanical stirring Methods 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 38
- 238000001816 cooling Methods 0.000 abstract description 14
- 238000001746 injection moulding Methods 0.000 abstract description 14
- 238000004040 coloring Methods 0.000 abstract description 7
- 101100397120 Arabidopsis thaliana PPA6 gene Proteins 0.000 abstract description 6
- 101150082829 gpa-6 gene Proteins 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 5
- 101100407670 Pseudoalteromonas haloplanktis pepQ gene Proteins 0.000 abstract description 4
- 101150031431 opa gene Proteins 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- LLMLGZUZTFMXSA-UHFFFAOYSA-N 2,3,4,5,6-pentachlorobenzenethiol Chemical compound SC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl LLMLGZUZTFMXSA-UHFFFAOYSA-N 0.000 abstract description 2
- 229960000892 attapulgite Drugs 0.000 abstract 8
- 229910052625 palygorskite Inorganic materials 0.000 abstract 8
- 239000002932 luster Substances 0.000 abstract 1
- 229920002292 Nylon 6 Polymers 0.000 description 104
- 239000002994 raw material Substances 0.000 description 12
- 239000004595 color masterbatch Substances 0.000 description 7
- 239000000835 fiber Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 208000006497 optic atrophy 6 Diseases 0.000 description 4
- 239000011550 stock solution Substances 0.000 description 4
- 239000004594 Masterbatch (MB) Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000010919 dye waste Substances 0.000 description 1
- 229920003247 engineering thermoplastic Polymers 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/548—Silicon-containing compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2272—Ferric oxide (Fe2O3)
Abstract
The invention relates to the technical field of PA6 material coloring, and discloses a preparation method of color PA6, which comprises the following steps: ATP (attapulgite) powder was dispersed in KOH solution for 24 hours, and then pigment (Fe) was added to the ATP suspension, respectively 2 O 3 、BiVO 4 And Al 6 Na 8 O 24 S 3 Si 6 ) Preparing a colored ATP suspension (RATP-Red, YATP-yellow and BATP-blue), mixing pigment powders with each other at a mass ratio of 1:1, preparing a mixed colored ATP (GATP-Green, PATP-purple and OATP-orange) suspension by the same method, and lyophilizing to obtain corresponding colored ATP suspensionATP powder, wherein the mass ratio of ATP to pigment is 2:1; the PA6 sample is prepared by slicing PA6, mixing and extruding dyed ATP (mass ratio of 100:1.5), and the color PA6 sample bars (RPA 6, YPA6, BPA6, GPA6, PPA6 and OPA 6) are prepared by cooling, granulating and injection molding. The preparation method of the color PA6 has the advantages of simple process, green and efficient preparation process, and good color and luster and excellent performance of the color PA6 product.
Description
Technical Field
The invention relates to the technical field of PA6 material coloring, in particular to a preparation method of color PA 6.
Background
PA6, also called nylon 6, is one of the most widely used engineering thermoplastics at present due to its excellent chemical stability and mechanical strength properties, as well as excellent properties such as high toughness, wear resistance, low density and low coefficient of friction. However, the PA6 fiber has the problems of poor pigment stability, low dye-uptake, environmental pollution (mainly referring to dye waste liquid in the dyeing process) and the like in the dyeing process, and along with the improvement of the environmental protection concept and the development trend of efficient utilization of the dye, the development is more concise, and the green dyeing method and the dyeing process have very important environmental protection and economic significance.
The traditional dyeing method of PA6 is to dye the fiber by using the diffusion, adsorption and other actions of the dye after spinning, but factors such as dyeing bath conditions, dye structural properties, dyeing and finishing technology and the like can seriously influence the dyeing effects such as color fastness, dyeing quantity, color feel and the like of the fiber fabric, and meanwhile, the traditional dyeing causes the defects of environmental pollution caused by dye liquor discharge, complex dyeing process, high resource consumption and the like. At present, the PA6 is colored in a stock solution coloring mode, the traditional dye bath link and complex dyeing procedures are avoided, and the method furthest reduces the resource consumption and the environmental pollution while obtaining the colored fibers with rich and uniform color and high color fastness. The common method for preparing the color PA6 product by the stock solution coloring method is a color master batch method, and the polymer is dyed by the color master batch method, so that the preparation of the polymer with rich and uniform color is realized, the preparation process flow is simplified, the resource consumption and the processing cost are greatly reduced, and the green efficient production of the colored polymer is satisfied.
However, the quality of the prepared PA6 color master batch is poor due to the relatively difficult color mixing, poor pigment dispersing effect, and the level of the master batch preparation technology, etc., so that the method has limitations to a certain extent, for example: patent CN112063166a discloses a preparation method of color PA6, which uses carbon black particles and a dispersing agent as colorants to prepare blue-phase black master batch and further prepare color PA6 slices and fibers, but the method still cannot avoid the defects of the color master batch method, such as single product color, poor pigment dispersing effect and the like, so that development of a greener environment-friendly, economical and efficient coloring mode is important for preparing color PA 6.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a preparation method of color PA 6. Solves the technical defects and problems of the prior art for preparing the color PA6 sample by coloring the stock solution.
(II) technical scheme
In order to achieve the above purpose, the present invention provides the following technical solutions: a color PA6 is prepared by dispersing ATP powder in KOH solution for 24 hr, and adding pigment (Fe 2 O 3 、BiVO 4 And Al 6 Na 8 O 24 S 3 Si 6 ) Preparing a staining ATP suspension (RATP, YATP and BATP); mixing pigment powder with each other in a mass ratio of 1:1, preparing mixed dyeing ATP (GATP, PATP and OATP) suspension according to the same method, and obtaining corresponding dyeing ATP powder by adopting a freeze drying mode, wherein the mass ratio of ATP to pigment is 2:1;
the color PA6 sample was prepared by slicing PA6, mixing and extruding dyed ATP (mass ratio of 100:1.5 and 100:3), and the color PA6 sample bars (RPA 6, YPA6, BPA6, GPA6, PPA6 and OPA 6) were prepared by cooling and granulating, and injection molding.
The present invention has the following advantages with respect to patent CN112063166 a:
(1) no PA6 color master batch is required to be prepared, and then the color PA6 is prepared through the color master batch;
(2) the pigment, the ATP and the PA6 are not interfered with each other, so that the dyed ATP with rich colors can be simply, conveniently and efficiently obtained by adjusting the proportion of different pigments, and the problem of difficult color mixing of color master batches in a stock solution coloring method is solved.
(3) ATP and pigment inorganic particles are uniformly dispersed in the PA6 matrix, so that the mechanical property of the color PA6 product is improved while the bright color of PA6 is endowed, and the heat-resistant stability of the product is ensured.
(4) The preparation flow is simple and efficient, and the PA6 samples with other colors can be prepared by blending the PA6 samples with different colors and extruding the mixture for the second time, so that the flexibility of preparing the color PA6 product is improved.
Under the dispersion and purification effects of KOH alkaline solution, ATP can effectively adsorb the inorganic pigment, thereby playing a role of pigment dispersion carrier, having good compatibility with PA6 matrix, and dyeing ATP can be uniformly dispersed in the PA6 matrix, so that the agglomeration of inorganic nano particles is avoided.
As a preferable technical scheme:
further, all the mixing was performed by mechanical mixing, and the sample mixture was extruded using a twin screw extruder at a temperature of about 250 ℃.
Further, the relative viscosity of the PA6 slice is about 2.5, and too high a relative viscosity of the PA6 slice can lead to uneven material mixing and poor melt flowability.
Further, the dispersion effect of ATP and pigment in the color PA6 sample reaches nano-scale dispersion, the elongation at break of the product sample bar reaches more than 300%, the maximum thermal weight loss temperature of the sample is about 450 ℃, the equilibrium water absorption is reduced to 4%, and the sample has high color fastness and stable color performance.
(III) beneficial effects
Compared with the prior art, the invention provides a preparation method of color PA6, which has the following beneficial effects:
1. compared with the traditional dyeing method and masterbatch method for preparing the color PA6, the method provided by the invention is green, environment-friendly, economical and efficient, simple in process operation and high in production efficiency.
2. According to the preparation method of the color PA6, the PA6 samples with various colors can be simply and quickly prepared through color mixing treatment, and the preparation of the color PA6 samples is more flexible and efficient through secondary extrusion and mixed extrusion.
3. The preparation method of the color PA6 has the advantages that the elongation at break of the color PA6 product reaches more than 300 percent, and the color PA6 product has high color fastness.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a TGA test curve of the products obtained in examples 1, 3, 5;
FIG. 2 is a graph showing the hygroscopicity/water absorption vs. time of the products obtained in examples 1, 3, 5, 7, 9, 11;
FIG. 3 is an SEM image of the product obtained in example 1;
FIG. 4 is an SEM image of the product obtained in example 3;
FIG. 5 is an SEM image of the product obtained in example 5;
FIG. 6 is a photograph of a product of the present invention;
FIG. 7 shows the theoretical formula of ATP according to the present invention: a Mg5Si8O20 (OH 2) 2 (OH) 4.4H2O graph;
FIG. 8 shows the crystal structure of ATP according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
In the following examples:
the detection method for the correlation performance of the prepared color PA6 sample in the following examples comprises the following steps:
mechanical properties: testing with reference to standard GB/T1040.1-2018;
color performance: color calibration mode is adopted by L;
water absorption performance: the test was performed with reference to standard GB/T1034-2008.
Example 1
The preparation method of the color PA6 comprises the following specific steps:
firstly, preparing raw materials:
PA6 slice (relative viscosity 2.5);
ATP powder;
Fe 2 O 3 ；
KOH solution (0.01 mol/L);
color PA6 samples (RPA 6-1) were prepared:
adding ATP powder into KOH solution, purifying and dispersing for 24h, and then adding Fe 2 O 3 The pigment powder was further dispersed for 24 hours, wherein the mass ratio of ATP to KOH solution was about1:20, wherein ATP and Fe 2 O 3 The mass ratio of the pigment is 2:1, and the suspension is freeze-dried to obtain RATP powder; mixing the PA6 slice and the RATP powder uniformly, preparing an RPA6 sample by melt extrusion of a double screw extruder, cooling, granulating, and performing injection molding to prepare an RPA6 spline, wherein the mass ratio of the PA6 slice to the RATP powder is 100:1.5, and the addition amount of pigment is 0.5% (other examples are modified according to the above).
Example 2
The preparation method of the color PA6 comprises the following specific steps:
firstly, preparing raw materials:
PA6 slice (relative viscosity 2.5);
ATP powder;
Fe 2 O 3 ；
KOH solution (0.01 mol/L);
color PA6 samples (RPA 6-2) were prepared:
adding ATP powder into KOH solution, purifying and dispersing for 24h, and then adding Fe 2 O 3 Dispersing pigment powder for 24 hr, freeze drying the suspension to obtain RATP powder, wherein the mass ratio of ATP to KOH solution is about 1:10, and the mass ratio of ATP to Fe is about 1:10 2 O 3 The mass ratio of the pigment is 2:1; uniformly mixing the PA6 slice and the RATP powder, preparing an RPA6 sample by melt extrusion of a double-screw extruder, cooling, granulating, and performing injection molding to prepare an RPA6 spline, wherein the mass ratio of the PA6 slice to the RATP powder is 100:3.
Example 3
The preparation method of the color PA6 comprises the following specific steps:
firstly, preparing raw materials:
PA6 slice (relative viscosity 2.5);
ATP powder;
BiVO 4 ；
KOH solution (0.01 mol/L);
color PA6 samples (YPA 6-1) were prepared again:
adding ATP powder into KOH solution, purifying and dispersing for 24h, and then adding BiVO 4 Dispersing pigment powder for 24 hr, freeze drying the suspensionDrying to obtain YATP powder, wherein the mass ratio of ATP to KOH solution is about 1:20, and the mass ratio of ATP to BiVO4 pigment is 2:1; mixing the PA6 slice and the YATP powder uniformly, preparing a YPA6 sample by melt extrusion of a double screw extruder, cooling, granulating, and performing injection molding to prepare YPA6 sample strips, wherein the mass ratio of the PA6 slice to the YATP powder is 100:1.5, and the addition amount of the pigment is 0.5%.
Example 4
The preparation method of the color PA6 comprises the following specific steps:
firstly, preparing raw materials:
PA6 slice (relative viscosity 2.5);
ATP powder;
BiVO 4 ；
KOH solution (0.01 mol/L);
color PA6 samples (YPA 6-2) were prepared again:
adding ATP powder into KOH solution, purifying and dispersing for 24h, and then adding BiVO 4 Dispersing pigment powder for 24 hr, freeze drying the suspension to obtain YATP powder, wherein the mass ratio of ATP to KOH solution is about 1:10, and the mass ratio of ATP to BiVO is about 1:10 4 The mass ratio of the pigment is 2:1; uniformly mixing the PA6 slice and the YATP powder, preparing a YPA6 sample by melt extrusion of a double-screw extruder, cooling, granulating, and performing injection molding to prepare YPA6 sample strips, wherein the mass ratio of the PA6 slice to the YATP powder is 100:3.
Example 5
The preparation method of the color PA6 comprises the following specific steps:
firstly, preparing raw materials:
PA6 slice (relative viscosity 2.5);
ATP powder;
Al 6 Na 8 O 24 S 3 Si 6 ；
KOH solution (0.01 mol/L);
prepare color PA6 sample (BPA 6-1):
adding ATP powder into KOH solution, purifying and dispersing for 24h, and then adding Al 6 Na 8 O 24 S 3 Si 6 Pigment powder continues to disperse24h, freeze-drying the suspension to obtain BATP powder, wherein the mass ratio of ATP to KOH solution is about 1:20, and the ATP to Al is 6 Na 8 O 24 S 3 Si 6 The mass ratio of the pigment is 2:1; uniformly mixing the PA6 slice and the BATP powder, preparing a BPA6 sample by melt extrusion of a double-screw extruder, cooling, granulating, and performing injection molding to prepare a BPA6 spline, wherein the mass ratio of the PA6 slice to the BATP powder is 100:1.5.
Example 6
The preparation method of the color PA6 comprises the following specific steps:
firstly, preparing raw materials:
PA6 slice (relative viscosity 2.5);
ATP powder;
Al 6 Na 8 O 24 S 3 Si 6 ；
KOH solution (0.01 mol/L);
prepare color PA6 sample (BPA 6-2):
adding ATP powder into KOH solution, purifying and dispersing for 24h, and then adding Al 6 Na 8 O 24 S 3 Si 6 Continuously dispersing the pigment powder for 24 hours, and freeze-drying the suspension to obtain BATP powder, wherein the mass ratio of ATP to KOH solution is about 1:10, and the mass ratio of ATP to Al6Na8O24S3Si6 pigment is 2:1; uniformly mixing the PA6 slice and the BATP powder, preparing a BPA6 sample by melt extrusion of a double-screw extruder, cooling, granulating, and performing injection molding to prepare a BPA6 spline, wherein the mass ratio of the PA6 slice to the BATP powder is 100:3.
Example 7
The preparation method of the color PA6 comprises the following specific steps:
firstly, preparing raw materials:
PA6 slice (relative viscosity 2.5);
ATP powder;
Al 6 Na 8 O 24 S 3 Si 6 ，BiVO 4 ；
KOH solution (0.01 mol/L);
prepare color PA6 sample (GPA 6-1):
adding ATP powder into KOH solution, purifying and dispersing for 24h, and then adding Al 6 Na 8 O 24 S 3 Si 6 And BiVO 4 Dispersing pigment powder for 24 hr, freeze drying the suspension to obtain GATP powder, wherein the mass ratio of ATP to KOH solution is about 1:20, and the mass ratio of ATP to Al is about 1:20 6 Na 8 O 24 S 3 Si 6 Pigment, biVO 4 The mass ratio of the pigment powder is 4:1:1; uniformly mixing the PA6 slice and the GATP powder, preparing a GPA6 sample by melt extrusion of a double-screw extruder, cooling, granulating, and performing injection molding to prepare GPA6 sample strips, wherein the mass ratio of the PA6 slice to the GATP powder is 100:1.5.
Example 8
The preparation method of the color PA6 comprises the following specific steps:
firstly, preparing raw materials:
PA6 slice (relative viscosity 2.5);
ATP powder;
Al 6 Na 8 O 24 S 3 Si 6 ，BiVO 4 ；
KOH solution (0.01 mol/L);
prepare color PA6 sample (GPA 6-2):
adding ATP powder into KOH solution, purifying and dispersing for 24h, and then adding Al 6 Na 8 O 24 S 3 Si 6 And BiVO 4 Dispersing pigment powder for 24 hr, freeze drying the suspension to obtain GATP powder, wherein the mass ratio of ATP to KOH solution is about 1:20, and the mass ratio of ATP to Al is about 1:20 6 Na 8 O 24 S 3 Si 6 Pigment, biVO 4 The mass ratio of the pigment powder is 4:1:1; uniformly mixing the PA6 slice and the GATP powder, preparing a GPA6 sample by melt extrusion of a double-screw extruder, cooling, granulating, and performing injection molding to prepare GPA6 sample strips, wherein the mass ratio of the PA6 slice to the GATP powder is 100:3.
Example 9
The preparation method of the color PA6 comprises the following specific steps:
firstly, preparing raw materials:
PA6 slice (relative viscosity 2.5);
ATP powder;
Al 6 Na 8 O 24 S 3 Si 6 ，Fe 2 O 3 ；
KOH solution (0.01 mol/L);
a color PA6 sample (PPA 6-1) was prepared:
adding ATP powder into KOH solution, purifying and dispersing for 24h, and then adding Al 6 Na 8 O 24 S 3 Si 6 With Fe 2 O 3 Dispersing pigment powder for 24 hr, freeze drying the suspension to obtain PATP powder, wherein the mass ratio of ATP to KOH solution is about 1:20, and the mass ratio of ATP to Al is about 1:20 6 Na 8 O 24 S 3 Si 6 Pigment, fe 2 O 3 The mass ratio of the pigment powder is 4:1:1; uniformly mixing the PA6 slice and the PATP powder, preparing a PPA6 sample by melt extrusion of a double-screw extruder, cooling, granulating, and preparing PPA6 sample bars by injection molding, wherein the mass ratio of the PA6 slice to the PATP powder is 100:1.5.
Example 10
The preparation method of the color PA6 comprises the following specific steps:
firstly, preparing raw materials:
PA6 slice (relative viscosity 2.5);
ATP powder;
Al 6 Na 8 O 24 S 3 Si 6 ，Fe 2 O 3 ；
KOH solution (0.01 mol/L);
a color PA6 sample (PPA 6-2) was prepared:
adding ATP powder into KOH solution, purifying and dispersing for 24h, and then adding Al 6 Na 8 O 24 S 3 Si 6 With Fe 2 O 3 Dispersing pigment powder for 24 hr, freeze drying the suspension to obtain PATP powder, wherein the mass ratio of ATP to KOH solution is about 1:20, and the mass ratio of ATP to Al is about 1:20 6 Na 8 O 24 S 3 Si 6 Pigment, fe 2 O 3 Mass of pigment powderThe ratio is 4:1:1; mixing the PA6 slice and the PATP powder uniformly, preparing a PPA6 sample by melt extrusion of a double-screw extruder, cooling, granulating, and performing injection molding to prepare PPA6 sample strips, wherein the mass ratio of the PA6 slice to the PATP powder is 100:3.
Example 11
The preparation method of the color PA6 comprises the following specific steps:
firstly, preparing raw materials:
PA6 slice (relative viscosity 2.5);
ATP powder;
BiVO 4 ，Fe 2 O 3 ；
KOH solution (0.01 mol/L);
a color PA6 sample (OPA 6-1) was prepared again:
adding ATP powder into KOH solution, purifying and dispersing for 24h, and then adding BiVO 4 With Fe 2 O 3 Dispersing pigment powder for 24 hr, freeze drying the suspension to obtain OATP powder, wherein the mass ratio of ATP to KOH solution is about 1:20, and the mass ratio of ATP to BiVO is about 1:20 4 Pigment, fe 2 O 3 The mass ratio of the pigment powder is 4:1:1; mixing the PA6 slice and the OATP powder uniformly, preparing an OPA6 sample by melt extrusion of a double-screw extruder, cooling, granulating, and performing injection molding to prepare OPA6 sample strips, wherein the mass ratio of the PA6 slice to the OATP powder is 100:1.5.
Example 12
The preparation method of the color PA6 comprises the following specific steps:
firstly, preparing raw materials:
PA6 slice (relative viscosity 2.5);
ATP powder;
BiVO 4 ，Fe 2 O 3 ；
KOH solution (0.01 mol/L);
a color PA6 sample (OPA 6-2) was prepared again:
adding ATP powder into KOH solution, purifying and dispersing for 24h, and then adding BiVO 4 With Fe 2 O 3 Dispersing pigment powder for 24 hr, freeze drying the suspension to obtain OATP powder, wherein ATP and KOH are dissolvedThe mass ratio of the liquid is about 1:20, and the ATP and BiVO are as follows 4 Pigment, fe 2 O 3 The mass ratio of the pigment powder is 4:1:1; mixing the PA6 slice and the OATP powder uniformly, preparing an OPA6 sample by melt extrusion of a double-screw extruder, cooling, granulating, and performing injection molding to prepare OPA6 sample strips, wherein the mass ratio of the PA6 slice to the OATP powder is 100:3.
The results of the performance tests of the color PA6 samples prepared in examples 1, 3, 5, 7, 9, 11 are shown in table 1:
TABLE 1
The color PA6 color performance test results obtained in examples 1, 3, 5, 7, 9, 11 are shown in table 2:
TABLE 2
Claims (7)
1. The preparation method of the color PA6 is characterized by comprising the following steps:
s1: firstly, dispersing ATP powder in KOH solution for 24 hours;
s2: then adding pigments into the ATP suspension respectively to prepare dyed ATP;
s3: and then the dyed ATP and the PA6 slice are mechanically mixed uniformly, and the color PA6 sample is prepared by melt extrusion at about 250 ℃, wherein the mass ratio of the PA6 slice to the dyed ATP is 100:1.5 and 100:3.
2. The method for preparing color PA6 according to claim 1, characterized in that: the pigment in the S2 is Fe 2 O 3 、BiVO 4 And Al 6 Na 8 O 24 S 3 Si 6 Wherein the mass ratio of ATP to pigment is 2:1, and wherein GATP, PATP and OATP are each made of Fe 2 O 3 、BiVO 4 And Al 6 Na 8 O 24 S 3 Si 6 The two pigments in (a) are mixed and prepared, and all the dyed ATP is obtained by a freeze drying mode.
3. The method for preparing color PA6 according to claim 1, characterized in that: the ATP powder is a natural nano material with strong adsorptivity, and needs to be dispersed and purified by alkali solution when preparing the dyed ATP.
4. The method for preparing color PA6 according to claim 1, characterized in that: the colors of the dyed ATP are six, the six dyed ATP are named according to the presented colors, and three mixed colors of dyed ATP are prepared by using the three primary color principle.
5. The method for preparing color PA6 according to claim 1, characterized in that: the S1 dispersing and mixing modes are mechanical stirring modes, and the dyeing ATP and the PA6 slice in the S3 are mixed by mechanical shaking.
6. The method for preparing color PA6 according to claim 1, characterized in that: in the step S1, the mass ratio of the ATP powder to the KOH solution is about 1:20, and a freeze drying mode is adopted to prepare a dyed ATP powder sample.
7. The method for preparing color PA6 according to claim 1, characterized in that: the dispersion effect of ATP and pigment in the color PA6 reaches nano-scale dispersion, the elongation at break of product sample bars reaches more than 300%, the temperature of the sample is 440-460 ℃ when the thermal weight loss rate of the sample is maximum, and the equilibrium water absorption rate is lower than 4%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310530825.3A CN116656121A (en) | 2023-05-11 | 2023-05-11 | Preparation method of color PA6 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310530825.3A CN116656121A (en) | 2023-05-11 | 2023-05-11 | Preparation method of color PA6 |
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| CN116656121A true CN116656121A (en) | 2023-08-29 |
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| CN202310530825.3A Pending CN116656121A (en) | 2023-05-11 | 2023-05-11 | Preparation method of color PA6 |
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| CN (1) | CN116656121A (en) |
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