Classifications

• • D—TEXTILES; PAPER
  • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
  • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
  • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
  • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
  • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
  • C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
  • C08G69/46—Post-polymerisation treatment
• • 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
  • C08K5/49—Phosphorus-containing compounds
  • C08K5/51—Phosphorus bound to oxygen
  • C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
  • C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
• • D—TEXTILES; PAPER
  • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
  • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
  • D01F1/00—General methods for the manufacture of artificial filaments or the like
  • D01F1/02—Addition of substances to the spinning solution or to the melt
  • D01F1/10—Other agents for modifying properties

Definitions

• the present invention relates to a process of treating chips of a specific polycarbonamide, namely polyhexamethylene adipamide, commonly termed nylon- 66, containing a phenyl derivative of hypophosphorous acid or salt thereof added during the polycondensation of the polymer-forming material to enhance the dye receptivity of filaments made therefrom.
• a specific polycarbonamide namely polyhexamethylene adipamide, commonly termed nylon- 66
• nylon- 66 commonly termed nylon- 66
• a commercially important polyamide of the aforesaid class is polyhexamethylene adipamide, known generally as nylon-66.
• nylon-66 polyhexamethylene diammoniumadipate (the salt of hexamethylene diamine and adipic acid) is heated under suitable polycondensation conditions to produce a fiber-forming polyamide having molecular weights represented by intrinsic viscosity values of about 0.3 to 1.3.
• Filaments are normally made from the fiber-forming polyamides by conventional melt spinning techniques. Unfortunately, such filaments have a limited aflinity to certain dyes. This limited afiinity of the filaments for dyes not only restricts the depth of obtainable color, but also greatly limits the range of dyes which can be employed.
• At least one of the above-defined phosphinic additives is introduced into the polymerization vessel with the nylon-forming substance for the purpose of enhancing the dye receptivity of filaments made from the ultimate polymer.
• the phosphinic additives generally are used in an amount of about 0.7 to 14.0 mol percent based on the weight of the nylon-forming substance With about 0.7 to 2.0 mol percent being preferred.
• the additive should be a member of the class of phosphinic compounds as above defined.
• metal phosphinates such as sodium phenylphosphinate, to a substantial extent do not improve the dye saturation level of nylon prepared in the presence thereof.
• benzenephosphinic acid or such acid which has been reacted with a suitable diamine such as hexarnethylene diamine to form hexamethylene diammoniumphenylphosphinate.
• hexamethylene diammoniumadipate and benzenephosphinic acid are charged to a polymerization vessel conventionally used in preparing nylon polymer.
• Nylon-forming reaction conditions are employed. That is, the reactants are heated at a temperature from about 180 C. to 300 C., and preferably from 200 C. to 295 C. until the product has a sufficiently high molecular weight to exhibit fiber-forming properties. This condition is reached when the nylon polymer possesses an intrinsic viscosity of at least 0.3.
• the resulting nylon polymer is castinto a ribbon which is quenched.
• the ribbon is diced into chips or flakes of the usual size.
• the chips are scoured. That is, they are contacted with a solvent so that soluble phosphinic compound is partly or totally removed from the chips. It has been found that Water or water containing a small amount of an alkaline substance gives excellent results as a material with which the chips can be scoured.
• the scouring can be accomplished in a variety of ways. In one procedure the chips can be soaked in or drenched with water.
• the scouring water has a pH of about 6 to 12.5, preferably 6 to 8, and a temperature of about 20 C. to 100 C. and higher.
• the scouring is carried out at or near the boiling point of water.
• The-scouring time normally will be between about 5 and minutes to reduce the soluble phosphinic compound to a minimum practical value.
• the scoured chips are dried in a suitable manner without degrading the polymer to a substantial extent.
• the chips can be dried in a vacuum oven at a temperature of 65 C. to 90 C. or centrifuged until .a moisture content of about two percent or lower is reached.
• the chips need not be dried completely, since the presence of some water can be used to create a static pressure head of steam normally maintained in melting Examples [-111 A stainless steel autoclave was charged with 406 parts of hexamethylene diammoniumadipate dissolved in an equal weight of water. A sufficient amount of acetic acid was added to stabilize the viscosity of the ultimate polymer at a relative viscosity of 34.
• the polymer flakes were divided into three equal portions. One portion of the flakes was placed in an extraction tray wrapped with an aluminum screen and suspended in a clean tank. The tank was rectangular with an open top having a capacity of approximately 50 gallons. The bottom and sides of the tank were jacketed for reception of steam. The tank was then filled with deionized water having a pH of 6.7. The Water was heated to boiling and this condition was continued for a period of 30 minutes. Thereafter, the steam was turned off and the water drained from the tank. This extraction procedure was then repeated twice after which the flakes were removed from the tank and transferred to a vacuum oven. The flakes were dried therein for a period'of 8 hours at 75 C; under vacuum.
• the thus-prepared water-scoured flakes were then spun into textile filaments using a conventional melt spinning apparatus.
• the air employed to solidify the filaments was analyzed for phosphorous content and was found to contain less than 0.05 ppm. phosphorous.
• the second portion of the flakes was spun into textile filaments by-passing the scouring and drying steps of the present invention.
• the air employed to solidify the filaments had a pungent obnoxious phosphorous-like odor.
• the third portion of the flakes was placed in a bag constructed of loosely woven nylon yarn.
• the bag was placed in boiling water containing 2.5 gms./ liter trisodium phosphate for 30 minutes.
• the pH of the water containing the trisodium phosphate was 11.4.
• the flake was then dried in a vacuum oven for 8 hours at 75 C.
• the thus-scoured flakes were spun into textile filaments using a conventional melt spinning apparatus.
• the air employed to solidify the filaments was analyzed for phosphorous content and was found to contain less than 0.05 p.p.m. phosphorous.
• the filaments prepared from the scoured flakes and the unscoured flakes were separately fabricated into 4 inch length samples of knit tubing. Tests were .then run on each of the fabric samples to determine their relative dye saturation levels. In the procedure used, each of the samples was dyed with equal concentrations of the commercial dyestutf Scarlet 4'RA (C.I. Acid Red 18). The dyeing was continued over a period of two hours in a bath having a liquor to fiber ratio of 40:1. A temperature of C. was maintained in the bath.
• the amount of .dye absorbed by each sample was determined by spectrophotometrically measuring the change in dye bath concentration, i.e., the difference between the original dye concentration in the bath and the exhausted dye concentration.- It was found that the amount of dye absorbed by the filaments spun from scoured flakes was substantially the same as the amount absorbed by the filaments spun from unscoured flakes. Values obtained averaged 1.95 percent dye absorbed for scoured sample-s vs. 2.08 percent for unscoured samples vs. 1.04 percent for samples not containing the phosphinic additive.
• Example IV Another batch of polymer was prepared as described in Example I. The flakes were poured into a tray and immersed in boiling deionized water. After 30 minutes the tank was drained and refilled with fresh deionized water. The temperature of the water was raised to the boiling point and the extraction process was repeated. After repeating the extraction a third time, the chips were removed from the tray and dried.
• a process of treating chips of polyhexamethylene adipamide polycondensed in the presence of about 0.7 to 14.0 mol percent based on the weight of the polymer forming substance of a dye-enhancing benzenephosphinic additive comprising the steps of:

Landscapes

• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Health & Medical Sciences (AREA)
• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Organic Chemistry (AREA)
• General Chemical & Material Sciences (AREA)
• Textile Engineering (AREA)
• Manufacturing & Machinery (AREA)
• Artificial Filaments (AREA)
• Compositions Of Macromolecular Compounds (AREA)

Priority Applications (8)

Applications Claiming Priority (1)

Publications (1)

Family

ID=22629169

Family Applications (1)

Country Status (6)

Citations (7)

• 0
  • BE BE628309D patent/BE628309A/xx unknown
• 1962
  • 1962-02-12 US US172773A patent/US3254059A/en not_active Expired - Lifetime
• 1963
  • 1963-01-28 GB GB3485/63A patent/GB979246A/en not_active Expired
  • 1963-02-07 CH CH152563A patent/CH425081A/fr unknown
  • 1963-02-11 DE DEM55751A patent/DE1260685B/de active Pending
  • 1963-02-11 DK DK63363AA patent/DK106753C/da active

Patent Citations (7)

Also Published As

Similar Documents