Polyarylene sulfide production method and polyarylene sulfide production apparatus

Patent metadata

Field	Value
Publication number	US-9908974-B2
Application number	US-201515303032-A
Country	US
Kind code	B2
Filing date	Apr 21, 2015
Priority date	Apr 30, 2014
Publication date	Mar 6, 2018
Grant date	Mar 6, 2018

Abstract

The present invention provides a production method and a production apparatus for a polyarylene sulfide (PAS), thus the formation of a floating polymer and the leakage of the floating polymer to the outside of the vessel in a washing step are prevented, to achieve steady production of the polymer with high quality, to improve the yield of the polymer and to reduce environmental load, wherein the floating polymer refers to a particles of the polymer which are floating on the surface of a washing solution, in the upper part of the inside of a washing vessel, as a result of the adhesion of a gas onto the surface of the particles of the polymer.
The present invention provides a production method for a PAS comprising step (I), performing polymerization, step (II), separating and collecting a polymer, step (III), washing a slurry, and step (IV), collecting the polymer after washing, wherein an aqueous medium is sprayed onto a PAS floating on the surface of the aqueous washing solution in the upper part of the inside of the washing vessel in step (III) (step (IIIa), washing a slurry using a counter current, and/or step (IIIb), treating a slurry with acid using a counter current, or the like); and a production apparatus for a PAS comprising a washing device (counter current washing device and/or a counter current contact/acid treatment device or the like) having an aqueous medium spray means.

First claim

The invention claimed is:

1. A production method for a polyarylene sulfide comprising the steps of:
(I) performing polymerization to produce a polymer via polymerization reaction on:
at least one type of a sulfur source selected from the group consisting of an alkali metal sulfide and an alkali metal hydrosulfide; and
a dihalo aromatic compound in an organic amide solvent;

(II) separating and collecting a polymer from a reaction solution containing the polymer produced by the polymerization reaction;
(III) washing a slurry of the collected polymer using a counter current by bringing the slurry into contact with at least one type of a washing solution selected from the group consisting of water, an organic solvent, and a mixed solution of water and an organic solvent, in a washing vessel, and/or;
treating a slurry comprising an acid using a counter current by bringing the slurry comprising the collected polymer and an acidic compound into contact with an aqueous washing solution, in the washing vessel; and

(IV) collecting the polymer after washing;
wherein, in step (III), polyarylene sulfide particles floating on a surface of the washing solution or the aqueous washing solution are reduced by separating and eliminating a gas adsorbed onto a surface of the polyarylene sulfide particles by spraying an aqueous medium to the polyarylene sulfide particles floating on the surface of the washing solution or the aqueous washing solution in an upper part of the inside of the washing vessel.

2. The production method for a polyarylene sulfide according to claim 1 , wherein the aqueous medium is sprayed by a nozzle device.

3. The production method for a polyarylene sulfide according to claim 2 , wherein the nozzle device comprises a plurality of nozzles.

4. The production method for a polyarylene sulfide according to claim 2 , wherein the nozzle device comprises a swivelable nozzle.

5. The production method for a polyarylene sulfide according to claim 1 , wherein the washing vessel is a wash-column.

6. The production method for a polyarylene sulfide according to claim 1 , wherein the acidic compound is hydrochloric acid or acetic acid.

7. The production method for a polyarylene sulfide according to claim 1 , wherein step (III) is repeatedly performed more than once.

8. The production method for a polyarylene sulfide according to claim 1 , wherein at least part of the slurry of the polymer contains a composition prepared outside the washing vessel.

9. The production method for a polyarylene sulfide according to claim 1 , wherein, in step (I), a polymerization reaction is performed on at least one type of a sulfur source selected from the group consisting of an alkali metal sulfide and an alkali metal hydrosulfide and a dihalo aromatic compound in an organic amide solvent in the presence of a phase separation agent at a temperature of from 170 to 290° C.

10. The production method for a polyarylene sulfide according to claim 1 , wherein a phase separation agent is added prior to step (II).

11. The production method for a polyarylene sulfide according to claim 9 , wherein the phase separation agent is at least one type selected from the group consisting of water, an organic carboxylic acid metal salt, an organic sulfonic acid metal salt, an alkali metal halide, an alkali earth metal halide, a phosphoric acid alkali metal salt, alcohols, and paraffin-based hydrocarbons.

12. The production method for a polyarylene sulfide according to claim 1 , wherein, prior to step (I), the production method comprises the steps of:
(A) dehydrating a mixture by heating and reacting a mixture containing:
an organic amide solvent;
a sulfur source containing an alkali metal hydrosulfide; and
an alkali metal hydroxide in an amount of from 0.95 to 1.05 mol per 1 mol of the alkali metal hydrosulfide;
and discharging at least part of a distillate containing water from inside a system containing the mixture to the outside of the system; and

(B) preparing a mixture by adding an alkali metal hydroxide and water as necessary to the mixture remaining inside the system after step (A) to adjust the mixture so that a total moles of an alkali metal hydroxide formed together with hydrogen sulfide produced at the time of dehydration, an alkali metal hydroxide prior to dehydration and the alkali metal hydroxide added after dehydration, is from 1.00 to 1.09 mol per 1 mol of the charged sulfur source and so that moles of water is from 0.02 to 2.0 mol per 1 mol of the charged sulfur source.

13. The production method for a polyarylene sulfide according to claim 1 , further comprising:
(V) re-separating a polyarylene sulfide particle by feeding the washing drainage discharged from the washing vessel to a polyarylene sulfide particle re-separation unit loaded with a filter to capture polyarylene sulfide particles and then re-separate and discharge the polyarylene sulfide particles from the filter.

14. The production method for a polyarylene sulfide according to claim 13 , wherein step (V) is repeatedly performed more than once.

15. The production method for a polyarylene sulfide comprising the step of:
washing a slurry of the polyarylene sulfide using a counter current by bringing the slurry into contact with at least one type of a washing solution selected from the group consisting of water, an organic solvent, and a mixed solution of water and an organic solvent, in a washing vessel; and/or
treating a slurry comprising the polyarylene sulfide and an acidic compound using a counter current by bringing the slurry comprising the polyarylene sulfide and the acidic compound into contact with an aqueous washing solution, in the washing vessel,
wherein polyarylene sulfide particles floating on a surface of the washing solution or the aqueous washing solution are reduced by separating and eliminating a gas adsorbed onto a surface of the polyarylene sulfide particles by spraying an aqueous medium to the polyarylene sulfide particles floating on the surface of the washing solution or the aqueous washing solution in an upper part of the inside of the washing vessel during washing.

Assignees

• Kureha Corp

Inventors

• Kobayashi Masanori
• Koizumi Tomoyoshi
• Matsuzaki Mitsuhiro
• Kawama Hirohito

Classifications

• C08G75/0254

  using metal sulfides · CPC title

• B01D29/11

  with bag, cage, hose, tube, sleeve or like filtering elements · CPC title

• C08G75/0213

  containing elements other than carbon, hydrogen or sulfur · CPC title

• B08B3/04

  Cleaning involving contact with liquid · CPC title

• B01D29/66

  by flushing, e.g. counter-current air-bumps · CPC title