Найлон 6 класса капролактам (CPL): высокая чистота белые хлопья экспортер
Nylon 6 Grade Caprolactam (CPL): High Purity White Flakes Exporter supplies monomeric caprolactam as white crystalline flakes intended for hydrolytic polymerisation to polyamide 6. The export specification for this grade is controlled through ISO 8660 permanganate absorption number, ISO 7060 solidification point, ISO 7059 UV absorbance, and ISO 760 Karl Fischer water content because these parameters govern ring-opening kinetics, terminal group balance, and colour stability in continuous polymerisation plants. Flake morphology, residual moisture, and trace metals are controlled before bagging and are verified on each export lot.
High-purity caprolactam is produced through Beckmann rearrangement of cyclohexanone oxime followed by neutralisation, extraction, hydrogenation, distillation, and melt crystallisation. The flake form is selected over prill or molten delivery when the receiving plant operates batch dissolution or extruder-fed polymerisation and requires proof of purity at the feeding point. Laboratory polymerisation checks are commonly used as a release test: a stirred autoclave charges 500 g of flake and 20 g distilled water under nitrogen, heats to 260 °C, and holds for 3 h before the polymer is extracted in boiling water and characterised. Lot acceptance is conditional on the resulting polyamide 6 viscosity number falling within the recipient’s target band, typically in the range of 2.4 to 2.8 relative viscosity when measured in 96% sulfuric acid according to ISO 307 or ASTM D789.
What Impurity Profiles Constrain Ring-Opening Polymerization?
Hydrolytic polymerisation of caprolactam is carried out in continuous VK tube reactors or agitated batch autoclaves at mass temperatures from 250 °C to 285 °C. Water at 2 wt% to 4 wt% initiates ring opening to 6-aminocaproic acid, after which step-growth condensation and ring-opening addition proceed simultaneously. Equilibrium conversion at 250 °C to 280 °C is conventionally accepted as approximately 90%, leaving cyclic dimer and cyclic trimer in the polymer melt at reported ranges of 6 wt% to 8 wt% and 2 wt% to 3 wt%, respectively, depending on residence time and temperature. These cyclic species are removed downstream by hot-water extraction or vacuum devolatilisation if residual levels must remain below 0.5 wt% for film, food-contact, or high-tenacity fibre grades.
Unsaturated and reducible impurities are critical because they absorb in the ultraviolet region and generate chromophores during polymerisation. The permanganate absorption number is determined on flake according to ISO 8660; a value below 10 000 s is generally treated as a rejection boundary for melt-spinning applications. UV absorbance measured on a 50% aqueous solution at 290 nm according to ISO 7059 is used to control carbonyl-containing and unsaturated trace components. Solidification point measured by ISO 7060 is expected at 68.8 °C or higher for dry high-purity material; depressions of 0.5 °C or more can indicate water, linear oligomers, or oxime carryover.
Metal ions introduce thermal oxidation and discoloration. Total iron in nylon 6 grade CPL is routinely controlled below 0.5 mg/kg, with total ash below 10 mg/kg, because ferrous and ferric species accelerate amide chain scission in the melt. Free alkalinity above 0.10 mmol/kg shifts the terminal group balance and must be neutralised before polymerisation; free acidity above the same order can deactivate heat stabiliser packages based on hindered phenol or copper iodide systems. Volatile bases, reported as ammonia, are held below 1.0 mg/kg to limit gas evolution in VK tube seals and spinning beams.
In continuous VK tube operation, caprolactam flake is fed through loss-in-weight feeders with feed accuracy of ±0.5% and melted in jacketed dissolution tanks. The temperature profile is divided into an upper ring-opening zone, a middle polycondensation zone, and a lower discharge zone. Feed variation larger than ±0.5% changes residence time and can shift the molecular weight distribution without changing the average relative viscosity. Published data for specific VK tube geometry is limited; however, field experience on single-stage continuous lines indicates that stable feed and water dosing are more important than minor specification variations within the high-purity range.
Flake Morphology, Moisture Sorption, and Conveying Behavior
White flake from melt crystallisation is specified with a thickness below 2 mm and a bulk density typically between 600 kg/m³ and 700 kg/m³. Fines smaller than 100 µm should be minimised because they increase dust explosion hazard and reduce hopper discharge consistency. Production-scale receiving data show that caking is most likely when flake temperature during unloading is below the ambient dew point or when relative humidity exceeds 60% for more than 24 h in non-sealed storage. Pre-drying with dry air at 30 °C to 40 °C is applied to reverse surface moisture before silo transfer, while desiccant dryers maintain storage headspace below 30% relative humidity.
Water content in the flake is controlled below 0.05 wt% by ISO 760. Moisture above 0.10 wt% alters the initial ring-opening rate in a VK tube and changes the final ratio of amine to carboxyl end groups, which affects dyeability and melt viscosity stability. The product is incompatible with strong oxidisers, concentrated acids in closed handling systems, and nitrosating agents because molten caprolactam can react exothermically or form nitrosamines. Storage above 45 °C is not recommended for extended periods because oxidation can increase APHA colour and reduce permanganate absorption number.
| Parameter | Method | Typical limit | Downstream significance |
|---|---|---|---|
| Caprolactam purity | GC-FID external standard | ≥ 99.9 wt% | Minimises chain transfer and oligomer formation |
| Solidification point | ISO 7060 | ≥ 68.8 °C | Confirms low water and impurity depression |
| Water content | ISO 760 | ≤ 0.05 wt% | Ensures predictable ring-opening rate |
| Permanganate absorption number | ISO 8660 | ≥ 10 000 s | Controls reducible impurities |
| UV absorbance at 290 nm | ISO 7059 | transmittance ≥ 75% in 50% aqueous solution | Limits chromophore precursors |
| Volatile bases as ammonia | ISO 8661 | ≤ 1.0 mg/kg | Reduces gas evolution in melt systems |
| Iron | ISO 6332 | ≤ 0.5 mg/kg | Prevents metal-catalysed degradation |
| APHA colour of molten sample | ASTM D1209 | ≤ 5 | Controls feedstock colour after heating |
The flake is melted and metered into continuous polymerisation units at rates that maintain residence times of 12 h to 24 h for textile-grade polymer. Agitation and temperature profile are adjusted to produce polyamide 6 with relative viscosity 2.4 to 2.8 as measured in 96% sulfuric acid according to ISO 307 or ASTM D789. End-group control is achieved with chain terminators such as acetic acid at levels below 0.5 wt% based on monomer mass. Published data for bespoke stabiliser formulations is limited and must be validated on the recipient’s specific reactor configuration.
When Melt Processing Requires Tight Relative Viscosity Control
Injection moulding grades of polyamide 6 derived from this caprolactam grade are typically produced at relative viscosity 2.8 to 3.4. Glass-reinforced compounds with 30 wt% short glass fibre are frequently compounded at RV 2.6 to 2.8 to retain mould fill pressure within the clamp force limits of 500 kN to 3 000 kN machines. Melt mass-flow rate according to ISO 1133-1:2022 at 235 °C and 2.16 kg is used as a supplementary process control, but it does not replace solution viscosity because it is less sensitive to terminal group imbalance. Free alkalinity in the flake above 0.10 mmol/kg can accelerate ring opening and produce broader molecular weight distributions; free acidity can consume copper-based stabiliser components.
Compounding on twin-screw extruders with L/D 40:1 and modular mixing elements at screw speeds of 250 min⁻¹ to 400 min⁻¹ disperses stabilisers, lubricants, and pigments. Barrel temperatures above 280 °C can reduce relative viscosity by 0.05 to 0.15 units through mechano-chemical chain scission, particularly when residence time exceeds 60 s at high shear. For this reason, the melt temperature is usually maintained at 240 °C to 275 °C for neat PA6, and the die pressure limit is set by the screen pack and gear pump arrangement rather than by the flake specification itself.
Molten PA6 produced from this caprolactam grade is filtered through sintered metal packs rated at 20 µm before filament spinning. Pressure rise across the pack at constant throughput indicates gel particles and cyclic agglomerates; a rise exceeding 10 bar per 8 h shift is typically investigated as a sign of thermal degradation or insufficient extraction. Spinning beam temperature is maintained at 260 °C to 275 °C for monofilament and multifilament operations, with quench air at 18 °C to 24 °C and 0.3 m/s to 0.5 m/s. Low volatile bases and low UV absorbance in the feedstock reduce the frequency of spinneret face deposits and broken filaments in high-speed winding.
Biaxially oriented PA6 film manufactured from this monomer grade is processed sequentially at machine-direction draw ratios of 3.2 to 4.0 and transverse-direction draw ratios of 3.5 to 4.5. Caprolactam impurities that reduce UV transmittance can generate haze and affect print adhesion after corona treatment. Residual cyclic dimer above 0.5 wt% in the polymer can migrate to the film surface and create roll-blocking during storage. The flake specification therefore links directly to film appearance and winding performance, even though the caprolactam itself is not present as such in the finished film.
Export Documentation Aligns with REACH and ISO 9001 Chain-of-Custody Clauses
Each export lot of Nylon 6 Grade Caprolactam (CPL): High Purity White Flakes Exporter is released with a certificate of analysis covering lot number, production date, retest date, and measured values against the specification. The certificate is issued under ISO 9001:2015 clause 8.5.2 lot traceability requirements. The safety data sheet follows REACH (EC 1907/2006) registration obligations for monomer substances and CLP (EC 1272/2008) classification for skin and eye irritation and short-term aquatic toxicity. Ocean freight uses 25 kg lined polyethylene bags on heat-treated wooden pallets or 500 kg to 1 000 kg bulk bags with moisture barrier liners. Customs declaration is completed under HS code 2933 71 00 for caprolactam.
| Document | Reference standard or regulation | Required data in polyamide 6 feedstock use |
|---|---|---|
| Certificate of analysis | ISO 9001:2015 clause 8.5.2 | Lot number, purity, water, PAN, UV absorbance, APHA colour |
| Safety data sheet | REACH (EC 1907/2006) Title IV | Hazard classification, exposure scenarios, handling boundaries |
| Food contact statement | FDA 21 CFR 177.1500 for downstream PA6 | Residual caprolactam migration limit in end article |
| Transport declaration | IMDG Code non-hazardous class | Molten or flake state, packaging code, net mass |
At receiving sites, flake should be stored in closed containers at 10 °C to 35 °C and below 50% relative humidity. When storage relative humidity exceeds 60%, pre-drying is required before melt handling; otherwise the water content can exceed 0.10 wt% and alter the amine-to-carboxyl end-group balance. The flake should not be blended with technical-grade caprolactam containing high oxime or high iron unless the recipient has validated the resulting polymer colour and UV stability. These constraints define the operational boundary for the product in continuous polymerisation and compounding.