Classifications

• • 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
  • C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
  • C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
  • C08G69/14—Lactams
  • C08G69/16—Preparatory processes

Definitions

• the present invention relates to a method for continuously decomposing higher aliphatic ⁇ -amino acids and a device used for the method.
• Aminoundecanoic acid and / or 12-Aminododecanoic acid (raw material or ⁇ -aminodecanoic acid) Mid (Nylon 11) and Pridedecaamide (Nylon 12) are useful because of their excellent low-temperature impact resistance and chemical resistance.
• Nylon ⁇ 1 and Nylon 12 from the ⁇ -amino acid are used to prepare a suspension of the ⁇ -amino acid powder in water.
• the suspension is heated to evaporate water to melt ⁇ -amino acid and to polycondensate the obtained ⁇ -amino acid melt.
• the ⁇ -amino acid granules need not be suspended in water, but can be continuously treated. It has been desired to develop a method and an apparatus for performing polycondensation efficiently and smoothly.
• the present invention has been completed based on the above background.
• the method of the present invention comprises the steps of: preparing a granule of a raw material of a polyamid * raw material comprising 11-amino decanoic acid and Z or 12-amino dodecanoic acid; Wrapping with an inert gas, supplying the sd powder wrapped with an inert gas to a melter without entraining a liquid, and immediately melting the sd powder.
• the following equipment is used. That is, a melting process for obtaining a melt by melting a powder material of a raw material made of 11-amino-undecane dumplings and a polyamide raw material consisting of no- or 12-7 minododenic acid.
• a small number of tubular polycondensation reactors connected to the melter via a pipe or without a pipe are used.
• the melter is a continuous polycondensation apparatus for higher aliphatic ⁇ -amino quinone, which is composed of the following small elements:
• An upper portion has a supply port for the powder and particles, and a lower portion has a bottom portion in the shape of a truncated cone or a pyramid, and the bottom portion of the bottom portion serves as a discharge port for the granules. container,
• FIG. 1 shows a side view of the apparatus of the present invention
• FIG. 2 shows a longitudinal sectional view of the melter.
• Figure 3 is a graph showing how long after the amino acid granules have been melted, polycondensation takes place.
• the apparatus of the present invention comprises two elements, a melter ⁇ and a polycondensation reactor B.
• the melter A melts a powder material of a raw material of polyamid comprising 11-amino-undecanoic acid and no or 12-amino-dodecanoic acid, and melts the melt of the raw material. To get it.
• a melter A is a polycondensation reactor B composed of small elements to be described later, which is used for immediately polycondensing the melt, and a conduit for flowing down the melt. Through or without the intermediary of the melter Reactor.
• FIG. 2 shows a state where the melter ⁇ and the polycondensation reactor ⁇ are connected without passing through a pipeline.
• the melter A has at least three small elements: a vessel 1, a piston 2, and a melting chamber 3.
• the container ⁇ has a supply port 5 for the powder 4 of the raw material of polyamide at an upper portion thereof, and a bottom portion 6 having a truncated cone or pyramid shape as a part of the main body 7 at a lower portion.
• the mounting portion 8 of the bottom 6 serves as a discharge port 9 for discharging the granular material 4 from the container 1.
• the piston 2 moves up and down substantially vertically on the vertical center line C at the outlet 9. The up and down movement is performed by any means, but is preferably performed by the air cylinder ⁇ 0.
• the guide 1 ⁇ is preferably a cylindrical shape having a cross-sectional shape and size substantially around the discharge port 9, so that at the height of the bottom 6, an inlet 12 for the granular material 4 is provided therearound. It is pierced.
• the guide 11 may also serve as the peripheral wall 13 of the outlet 9 depending on the case, and may further form an extension 14 of the outlet 9.
• the melting chamber 3 is a chamber for melting the granular material, and is provided continuously below the discharge port 9, and its cross-sectional area S i is equal to the cross-sectional area S of the discharge port 9. Greater than two. And inside it, a grid-like mature plate "15" is built.
• the cross-sectional area S i in the above means an arbitrary cross-sectional area at an upper and lower position between the outlet 9 and the mat 15. Therefore, it can be said that the upper body 6 in the melting chamber has, for example, a frustoconical shape.
• the lower body 17 below the hot plate 15 is connected to the bottom 18 of the squeezing structure to facilitate the collection of the melt.
• a pipe 19 connected thereto is connected to the polycondensation reactor.
• the method of the present invention using the above device is carried out as follows.
• the raw material of the polyamide to be used in the present invention is at least one kind of ⁇ -amino acid selected from ⁇ -amino-, decanoic acid and 12-amino-dodecanoic acid. It is a granular material.
• This raw material is solid at room temperature, and is industrially obtained as a powder.
• the use of a powder preferably having an average particle size of 0.05 to 4 among the powders and granules exerts the effects of the present invention remarkably.
• the first operation of the present invention is to wrap the raw material granules with an inert gas. Wrapping here means placing the powder and granules in a room or container that is shielded from the atmosphere, putting the inert gas inside the container and expelling the air in the container and filling the voids between the powder and particles with the inert gas. And. Such an operation can be carried out in the container 1, but is preferably carried out in a separately provided container (not shown) before supplying the powder to the container 1.
• the second operation of the present invention is to melt the powder and granules wrapped in an inert gas without entraining a liquid therein.
• the powder 4 is supplied into the container 1 from the supply port 5 of the container ⁇ , and the powder 4 filled in the container ⁇ is pushed into the melting chamber 3 by the biston 2.
• the operation of pushing the granular material 4 into the melting chamber 3 is performed by vertically moving the piston 2 by operating the air cylinder 10. When the piston 2 is moved upward, the granular material 4 enters the guide from the inlet 12 drilled below the guide 1, and the powder 4 moves downward due to the downward movement of the piston 2.
• the powder is supplied to the melting chamber 3 through the discharge port 9 and the powder is supplied to the inlet ⁇ 2 when the bottom 6 of the container ⁇ is shaped like a cone or pyramid.
• the cross-sectional area S i of the melting chamber 3 which is automatically performed is larger than the cross-sectional area S 2 of the discharge port 9. Therefore, the amount of the granular material in the discharge port 9 falls in the melting chamber 3 by an amount corresponding to the amount melted by the grid-shaped hot plate ⁇ 5, falls naturally, and accumulates on the hot plate ⁇ 5. To Then it melts upon request.
• the melt from the melted granules is collected at the bottom 18 and sent to the polycondensation reactor via line 19.
• the melt must reach the polycondensation apparatus within 20 minutes, preferably within 5 minutes after the melt is formed. Is the subject of the present invention.
• the ⁇ -amino acid forms a polymer in the melting chamber due to the progress of the polycondensation reaction after the above-mentioned time, and the melt is transferred from the melting chamber to the polycondensation reactor. This makes it impossible. This phenomenon cannot be observed in the conventionally known method of polymerizing a liquid by entraining the liquid, which suppresses the progress of the polymerization of the liquid (water).
• the melt is subjected to polycondensation at 220 to 290 ° C., preferably 240 to 270 ° C. under normal pressure, pressurization and reduced pressure. Then, a polyamide is obtained. This is once made into pellets by a well-known method, or it is made into a product directly as a fiber.
• the entrained liquid does not need to be removed in the polycondensation reactor, which has the effect of reducing the heating energy in the polycondensation reactor. .
• the ripening temperature of the melter is set at 230, and the supplied ⁇ -aminot * decane is brought into contact with the hot plate grid and melted by the periodic up and down operation of the piston.
• the melt takes about 30 seconds and is supplied to the decompression / combination f ss;
• the ripening jacket of the polycondensation reactor is maintained at 260 in the upper stage, 250 in the middle stage, and 240 ° in the lower stage.
• the solution is spun out of the polycondensation reactor into a strand at a discharge rate of 27.3 K3 hr by a quantitative pump. ⁇ Cooling bath
• the product is cooled by the heat and becomes a pellet-shaped product.
• the viscosity of the melt is low enough to be transferred from the melter to the polycondensation reactor, and is supplied stably and easily from the melter to the polycondensation reactor. I was able to do this.

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• Chemical & Material Sciences (AREA)
• Health & Medical Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Organic Chemistry (AREA)
• Polyamides (AREA)

Priority Applications (2)

Applications Claiming Priority (2)

Publications (1)

Family

ID=16246006

Family Applications (1)

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• 1981
  • 1981-11-26 JP JP56189717A patent/JPS5891722A/ja active Granted
• 1982
  • 1982-11-25 US US06/525,047 patent/US4546171A/en not_active Expired - Fee Related
  • 1982-11-25 BR BR8207994A patent/BR8207994A/pt not_active IP Right Cessation
  • 1982-11-25 WO PCT/JP1982/000450 patent/WO1983001954A1/ja not_active Ceased
  • 1982-11-25 EP EP82903472A patent/EP0094435B1/en not_active Expired
  • 1982-11-25 DE DE8282903472T patent/DE3276237D1/de not_active Expired

Patent Citations (1)

Non-Patent Citations (1)

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