WO2018164010A1

WO2018164010A1 - Device for producing polyarylene sulfide

Info

Publication number: WO2018164010A1
Application number: PCT/JP2018/008128
Authority: WO
Inventors: 崇之木村; 義宏一ノ瀬; 精孝 ▲但▼野; 小林　正則
Original assignee: 株式会社クレハ
Priority date: 2017-03-06
Filing date: 2018-03-02
Publication date: 2018-09-13

Abstract

Provided is a device for producing polyarylene sulfide (hereinafter, PAS), wherein the corrosion resistance of a valve provided in a supply path for supplying a reaction tank with a sulfur source which is a raw material can be improved to reduce the replacement frequency of the valve. The device for producing PAS according to the present invention is provided with: a reaction tank for producing PAS by polymerizing a sulfur source and a dihalo aromatic compound in an organic polar solvent; a supply path communicating with the reaction tank, and supplying the sulfur source to the reaction tank; and one or more valves provided in the supply path, and opening and closing the supply path. At least one of the valves is made of a zirconium-containing material. Preferably, only the valve closest to the reaction tank among the one or more valves is made of the zirconium-containing material. In addition, preferably, the content of zirconium in the zirconium-containing material is 95-100 mass%.

Description

Polyarylene sulfide production equipment

The present invention relates to an apparatus for producing polyarylene sulfide.

Polyarylene sulfide (hereinafter also referred to as “PAS”) represented by polyphenylene sulfide (hereinafter also referred to as “PPS”) has heat resistance, chemical resistance, flame resistance, mechanical strength, electrical properties, and dimensions. Engineering plastic with excellent stability. PAS can be molded into various molded products, films, sheets, fibers, etc. by general melt processing methods such as extrusion molding, injection molding, compression molding, etc., so electrical equipment, electronic equipment, automotive equipment, packaging materials, etc. Widely used in a wide range of technical fields.

Examples of the method for producing PAS include a method for producing PAS by polymerizing a sulfur source and a dihaloaromatic compound in an organic amide solvent (for example, Patent Documents 1 and 2).

JP 2014-47218 A International Publication No. 2006/046748

In the manufacture of PAS, raw materials that are highly corrosive to metal and wearable may be used, so that high corrosion resistance is required for the metal members constituting the reaction tank in the PAS manufacturing apparatus. On the other hand, the valve provided in the supply path for supplying the raw material sulfur source to the reaction tank is one in which the reaction solution does not directly pass through. in use.

However, according to the study by the inventors, even a valve that does not allow the reaction solution to pass directly may be corroded by a sulfur-containing atmosphere such as hydrogen sulfide generated in the reaction vessel, and particularly close to the reaction vessel. Since the valve is easily corroded by the sulfur-containing atmosphere, the valve needs to be replaced periodically.

This invention is made in view of said subject, Comprising: The frequency which replace | exchanges the said valve is reduced by improving the corrosion resistance of the valve provided in the supply path which supplies the sulfur source which is a raw material to a reaction tank. An object of the present invention is to provide an apparatus for manufacturing a PAS that can be used.

The present inventors have found that the above object can be achieved by using a valve formed of a zirconium-containing material, and have completed the present invention.

The PAS manufacturing apparatus according to the present invention comprises:
A reaction vessel for polymerizing a sulfur source and a dihaloaromatic compound in an organic polar solvent to produce PAS;
A supply path communicating with the reaction tank and supplying the sulfur source to the reaction tank;
At least one valve provided in the supply path for opening and closing the supply path;
With
At least one of the valves is formed from a zirconium-containing material.

In the PAS manufacturing apparatus according to the present invention, it is preferable that a valve closest to the reaction vessel among the at least one valve is formed of the zirconium-containing material.

In the PAS manufacturing apparatus according to the present invention, the zirconium content in the zirconium-containing material is preferably 95 to 100% by mass.

ADVANTAGE OF THE INVENTION According to this invention, the manufacturing apparatus of PAS which can reduce the frequency which replace | exchanges the said valve | bulb by improving the corrosion resistance of the valve | bulb provided in the supply path which supplies the sulfur source which is a raw material to a reaction tank is provided. be able to.

It is typical sectional drawing which shows one Embodiment of the manufacturing apparatus of PAS which concerns on this invention.

The manufacturing apparatus according to the present invention can be applied to a PAS manufacturing apparatus in which a corrosive material such as strong alkali is introduced into a reaction tank to perform a polymerization reaction. Below, one Embodiment of the manufacturing apparatus of PAS which concerns on this invention with the method to manufacture PAS is described.

I. PAS production method The method for producing PAS is not particularly limited as long as the gist of the present invention is not impaired, and generally, a charging step, a polymerization step (a two-stage polymerization step comprising a pre-stage polymerization step and a post-stage polymerization step) And a method of further comprising a dehydration step.

1. Dehydration step The dehydration step is a step of discharging a distillate containing water from the reaction system during the polymerization reaction, which contains a mixture containing an organic polar solvent and a sulfur source, before the preparation step.

The polymerization reaction between the sulfur source and the dihaloaromatic compound is affected by being accelerated or inhibited by the amount of water present in the polymerization reaction system. Therefore, the dehydration step is not indispensable as long as the water content does not inhibit the polymerization reaction, but it is preferable to reduce the water content in the polymerization reaction system by performing a dehydration treatment before the polymerization.

In the dehydration step, it is preferable to perform dehydration by heating in an inert gas atmosphere. A dehydration process is performed within a reaction tank, and the distillate containing water is discharged | emitted out of a reaction tank. The water to be dehydrated in the dehydration step is hydrated water contained in each raw material charged in the dehydration step, an aqueous medium of an aqueous mixture, water by-produced by a reaction between the raw materials, and the like.

The heating temperature in the dehydration step is not particularly limited as long as it is 300 ° C. or less, and is preferably 100 to 250 ° C. The heating time is preferably 15 minutes to 24 hours, and more preferably 30 minutes to 10 hours.

In the dehydration process, dehydration is performed until the water content falls within a predetermined range. That is, in the dehydration step, it is desirable to dehydrate until the amount of water is preferably 0 to 2 mol, more preferably 0.5 to 1.8 mol with respect to 1 mol of the effective sulfur source described later. When the amount of water becomes too small in the dehydration step, water may be added to adjust the desired amount of water in the preparation step prior to the polymerization step.

2. Preparation Step The preparation step is a step of preparing a mixture containing an organic polar solvent, a sulfur source, a dihaloaromatic compound, and water. A mixture charged in the charging step is also referred to as a “charged mixture”.

When the dehydration step is performed, the amount of sulfur source in the charged mixture (hereinafter also referred to as “the amount of charged sulfur source” (effective sulfur source)) was volatilized in the dehydration step from the molar amount of the sulfur source charged in the dehydration step. It can be calculated by subtracting the molar amount of hydrogen sulfide.

When performing the dehydration step, an alkali metal hydroxide and water can be added to the mixture remaining in the system after the dehydration step, if necessary. In particular, the alkali metal hydroxide is added in consideration of the amount of hydrogen sulfide generated during dehydration and the amount of alkali metal hydroxide generated during dehydration.

In the charged mixture, the amount of each of the organic polar solvent and the dihaloaromatic compound used is set, for example, within the range shown in the following description regarding the polymerization step with respect to 1 mol of the charged sulfur source.

3. Polymerization step In the polymerization step, PAS is produced by polymerizing a sulfur source and a dihaloaromatic compound in an organic polar solvent. The polymerization reaction in the main polymerization step is performed by heating a mixture containing the sulfur source and the dihaloaromatic compound. In order to obtain a higher viscosity PAS, the polymerization reaction may be carried out in two or more stages. The polymerization reaction is preferably, for example, a pre-polymerization reaction between the sulfur source and the dihaloaromatic compound. The pre-stage polymerization reaction is a polymerization reaction in which a mixture containing the sulfur source and the dihaloaromatic compound is heated to start the polymerization reaction, and a prepolymer having a dihaloaromatic compound conversion rate of 50% or more is generated.

In the polymerization reaction, it is preferable to carry out the polymerization reaction under heating at a temperature of 170 to 300 ° C. from the viewpoint of the efficiency of the polymerization reaction. The polymerization temperature in the polymerization reaction is more preferably in the range of 180 to 280 ° C. in order to suppress side reactions and decomposition reactions. In particular, in the pre-stage polymerization reaction, from the viewpoint of the efficiency of the polymerization reaction, the polymerization reaction is started under heating at a temperature of 170 to 270 ° C., and a prepolymer having a dihaloaromatic compound conversion rate of 50% or more can be generated. preferable. The polymerization temperature in the pre-stage polymerization reaction is preferably selected from the range of 180 to 265 ° C. in order to suppress side reactions and decomposition reactions.

In the main polymerization step, the conversion rate of the dihaloaromatic compound in the pre-stage polymerization reaction is preferably 50 to 98%, more preferably 60 to 97%, still more preferably 65 to 96%, and particularly preferably 70 to 95%. . The conversion rate of the dihaloaromatic compound is calculated based on the amount of the dihaloaromatic compound remaining in the reaction mixture by gas chromatography and based on the remaining amount, the charged amount of the dihaloaromatic compound, and the charged amount of the sulfur source. Can do.

The polymerization reaction in the main polymerization step may be performed batchwise or continuously. For example, supply of at least an organic polar solvent, a sulfur source, and a dihaloaromatic compound, production of PAS by polymerization of the sulfur source and the dihaloaromatic compound in the organic polar solvent, and recovery of a reaction mixture containing PAS; , The polymerization reaction can be carried out continuously by carrying out in parallel.

In addition, as an organic polar solvent, a sulfur source, and a dihalo aromatic compound, what is normally used in manufacture of PAS can be used. Each of the organic polar solvent, the sulfur source, and the dihaloaromatic compound may be used singly or in combination of two or more as long as the PAS can be produced.

Examples of the organic polar solvent include an organic amide solvent; an aprotic organic polar solvent composed of an organic sulfur compound; and an aprotic organic polar solvent composed of a cyclic organic phosphorus compound. Examples of the organic amide solvent include amide compounds such as N, N-dimethylformamide and N, N-dimethylacetamide; N-alkylcaprolactam compounds such as N-methyl-ε-caprolactam; N-methyl-2-pyrrolidone (hereinafter, “ NMP ”), N-alkylpyrrolidone compounds such as N-cyclohexyl-2-pyrrolidone or N-cycloalkylpyrrolidone compounds; N, N-dialkylimidazolidinones such as 1,3-dialkyl-2-imidazolidinone Compounds; tetraalkylurea compounds such as tetramethylurea; hexaalkylphosphate triamide compounds such as hexamethylphosphate triamide, and the like. Examples of the aprotic organic polar solvent composed of an organic sulfur compound include dimethyl sulfoxide and diphenyl sulfone. Examples of the aprotic organic polar solvent comprising a cyclic organophosphorus compound include 1-methyl-1-oxophosphorane. Among these, organic amide solvents are preferable in terms of availability, handling, and the like, and N-alkylpyrrolidone compounds, N-cycloalkylpyrrolidone compounds, N-alkylcaprolactam compounds, and N, N-dialkylimidazolidinone compounds are more preferable. NMP, N-methyl-ε-caprolactam, and 1,3-dialkyl-2-imidazolidinone are even more preferred, and NMP is particularly preferred. The amount of the organic polar solvent used is preferably from 1 to 30 mol, more preferably from 3 to 15 mol, based on 1 mol of the sulfur source from the viewpoint of the efficiency of the polymerization reaction.

Examples of the sulfur source include alkali metal sulfides, alkali metal hydrosulfides, and hydrogen sulfide, and alkali metal sulfides and alkali metal hydrosulfides are preferable. The sulfur source can be handled in the form of, for example, an aqueous slurry or an aqueous solution, and is preferably in the state of an aqueous solution from the viewpoint of handling properties such as meterability and transportability. Examples of the alkali metal sulfide include lithium sulfide, sodium sulfide, potassium sulfide, rubidium sulfide, and cesium sulfide. Examples of the alkali metal hydrosulfide include lithium hydrosulfide, sodium hydrosulfide, potassium hydrosulfide, rubidium hydrosulfide, and cesium hydrosulfide.

Dihaloaromatic compounds include o-dihalobenzene, m-dihalobenzene, p-dihalobenzene, dihalotoluene, dihalonaphthalene, methoxy-dihalobenzene, dihalobiphenyl, dihalobenzoic acid, dihalodiphenyl ether, dihalodiphenyl sulfone, dihalodiphenyl sulfoxide Dihalodiphenyl ketone, and the like. Halogen atoms refer to fluorine, chlorine, bromine and iodine atoms, and the two halogen atoms in the dihaloaromatic compound may be the same or different. Among these, p-dihalobenzene, m-dihalobenzene, and a mixture of both are preferable in terms of availability, reactivity, and the like, p-dihalobenzene is more preferable, and p-dichlorobenzene (hereinafter also referred to as “pDCB”). Particularly preferred. The amount of the dihaloaromatic compound to be used is preferably 0.90 to 1.50 mol, more preferably 0.92 to 1.10 mol, still more preferably with respect to 1 mol of the charged sulfur source. 0.95 to 1.05 mol. When the amount used is within the above range, a decomposition reaction is unlikely to occur, a stable polymerization reaction can be easily performed, and a high molecular weight polymer is easily generated.

4). Post-treatment process (separation process, washing process, recovery process, etc.):
As a method for producing PAS, the post-treatment step after the polymerization reaction can be performed by a conventional method. For example, after the polymerization reaction is completed, the slurry containing the produced PAS polymer is kept in a high temperature state or cooled, and then diluted with water or the like as desired, and then the PAS polymer is filtered by sieving or the like, Next, the separated PAS polymer is washed with an organic solvent such as the same polar solvent as the polymerization solvent, an organic solvent such as ketones (for example, acetone), alcohols (for example, methanol), hot water, and filtration. Thus, a recovery step for recovering PAS can be performed. The produced PAS can be treated with a salt such as acid or ammonium chloride. According to this method, since a granular polymer can also be generated, it is possible to separate the granular polymer from the reaction liquid by a method of sieving using a screen, so that it can be easily separated from by-products and oligomers. preferable.

II. PAS manufacturing apparatus The PAS manufacturing apparatus according to the present invention communicates with a reaction tank for polymerizing a sulfur source and a dihaloaromatic compound in an organic polar solvent to produce polyarylene sulfide, and the reaction tank. A supply path for supplying the sulfur source to the tank, and at least one valve provided in the supply path for opening and closing the supply path, wherein at least one of the valves is made of a zirconium-containing material. Is formed. Hereinafter, description will be given with reference to the drawings.

1. Reaction Tank As shown in FIG. 1, a PAS manufacturing apparatus 100 according to an embodiment of the present invention includes a reaction tank 1. As a PAS manufacturing method performed by applying the PAS manufacturing apparatus 100, the reaction tank 1 is used, and at least the charging process and the polymerization process are performed in the reaction tank 1 (therefore, the reaction tank 1 is a “polymerization tank” or Sometimes referred to as “polymerization can”), and if desired, a dehydration step is performed.

As the reaction tank 1 provided in the PAS manufacturing apparatus 100, the same shape, structure, size, etc. as in the reaction tank conventionally provided and used in the PAS manufacturing apparatus can be applied, and the same material is used. Can be formed from That is, the reaction vessel 1 usually has a structure including a cylindrical body portion 11, a lid portion 12 and a bottom portion 13. In the reaction tank 1, a stirring blade 21 and a stirring shaft 22 are usually inserted, and one or a plurality of baffles (baffle plates) 3 are provided on the inner peripheral wall. The agitation shaft 22 is connected to an electric motor (not shown) disposed above the reaction tank 1 and is driven to rotate.

[Cover]
The lid 12 of the reaction tank 1 is usually a bowl-shaped member that is connected to and attached to the upper part of the cylindrical body 11, and is provided with a hole through which the stirring shaft 22 described above is inserted. . As will be described in detail later, the reaction vessel 1 includes raw material monomers and other materials (alkali metal hydroxides and the like. In addition, the raw material monomers and other materials are collectively referred to as “various”. Or a plurality of supply passages 4 (sometimes referred to as “supply nozzles”) for charging the reaction tank 1 into the interior of the reaction tank 1 ( In FIG. 1, one supply path 4 is shown as a supply path for supplying the sulfur source to the reaction tank 1). The lid 12 may be provided with an openable / closable opening or the like so that the inside of the reaction tank 1 can be inspected, cleaned, and the like. The opening that can be opened and closed is usually larger in diameter than the supply path 4. If desired, the lid portion 12 may be provided with a required number of baffle fixing portions for suspending and fixing the baffles 3 arranged in the reaction tank 1.

〔bottom〕
The bottom 13 of the reaction tank 1 is a generally bowl-shaped member that is connected to and attached to the lower part of the cylindrical body 11. The bottom 13 is usually provided with a discharge pipe 131 (also referred to as a “discharge nozzle”) for discharging the PAS polymer produced by the polymerization reaction, and various raw materials are charged into the reaction tank 1 as desired. There is a case where a supply path is provided.

(Cylindrical body)
The cylindrical body 11 of the reaction tank 1 constitutes a main part of the reaction tank 1, and a charging process, a polymerization process, and a dehydration process are performed therein if desired. A stirring blade 21 and a stirring shaft 22 and a baffle (baffle plate) 3 are usually arranged inside the cylindrical body 11. In FIG. 1, the baffle 3 is directly attached to the inner wall of the cylindrical body 11. However, the baffle 3 may be supported by a baffle support protruding from the inner wall of the reaction tank 1, specifically, the inner wall of the cylindrical body 11, or as mentioned above, You may make it hang and fix from the cover part 12. FIG.

[Other parts]
Usually, other required members are connected to the reaction tank 1 including the cylindrical body portion 11, the lid portion 12, and the bottom portion 13. The electric motor that rotates the agitation shaft 22 described above is an example. Further, for example, a heat exchange jacket for adjusting the temperature of the reaction vessel 1, particularly the cylindrical body 11, is an outer peripheral surface of the reaction vessel 1. May be provided so as to surround. Further, for example, various pipes may be provided for the purpose of transferring various raw materials and the like, PAS polymer to be produced, circulation of a heat medium and / or refrigerant, and the like.

As a material for forming the reaction tank 1, since the polymerization reaction of PAS is carried out in a high temperature, high pressure and high alkali environment, a material excellent in strength and chemical resistance in a high temperature environment is required. Specific examples include corrosion resistant metals such as titanium materials (may be titanium alloys), zirconium materials (may be zirconium alloys), special austenitic steels [Carpenter (registered trademark), etc.], and these plate-like materials, A laminate in which a corrosion-resistant metal such as titanium or zirconium is provided on the inner surface of the reaction vessel 1, such as a titanium-coated steel material or a clad material, is used. The thickness and size of the corrosion-resistant metal plate material (including clad material) are appropriately determined as necessary. The same applies to materials forming members such as the baffle 3 disposed in the reaction tank 1.

2. Supply Path As shown in FIG. 1, the PAS manufacturing apparatus 100 includes a supply path 4. The supply path 4 communicates with the reaction tank 1 and supplies a sulfur source to the reaction tank 1. The supply path 4 is connected to the lid portion 12 of the reaction tank 1 as shown in FIG. 1, for example. In addition to the supply path 4, the PAS manufacturing apparatus 100 includes one or a plurality of supply paths for introducing various raw materials such as raw material monomers and alkali metal hydroxide into the reaction tank 1 (not shown). )

The diameter, length, and thickness of the supply path 4 can be appropriately set in consideration of the type of the sulfur source supplied from the supply path 4, the input amount to the reaction tank 1, the strength required for the supply path 4, and the like. . The supply path 4 is preferably formed from a corrosion-resistant material such as a titanium material or a zirconium material.

3. Valve As shown in FIG. 1, the PAS manufacturing apparatus 100 includes a valve 5. The valve 5 is provided in the supply path 4 and opens and closes the supply path 4. Although FIG. 1 shows the case where one valve is provided in the supply path 4, a plurality of valves may be provided in the supply path 4. By opening the valve 5, the sulfur source is supplied to the reaction tank 1 through the supply path 4, and by closing the valve 5, the supply of the sulfur source to the reaction tank 1 through the supply path 4 is completed.

The shape of the valve 5 is not particularly limited as long as the sulfur source can be supplied to the reaction tank 1. As the valve 5, for example, a butterfly valve, a ball valve, a diaphragm valve, a globe valve, a plug valve, a ball valve, or the like can be used. In the present embodiment, a ball valve is preferable from the viewpoint of operability, flow rate adjustability, and the like.

The valve 5 is made of a zirconium-containing material. Thereby, even if a sulfur-containing atmosphere such as hydrogen sulfide generated in the reaction tank 1 comes into contact with the valve 5, the valve 5 is hardly corroded. When a plurality of valves are provided in the supply path 4, at least one of these valves is made of a zirconium-containing material, and preferably the valve closest to the reaction vessel 1 among these valves. Is formed from the zirconium-containing material. Among these valves, in particular, the valve closest to the reaction vessel is likely to corrode due to the sulfur-containing atmosphere, and therefore needs to be replaced periodically.If the valve is formed from the zirconium-containing material, The frequency of exchange can be effectively reduced.

Since the valve 5 in the present embodiment is provided in the supply path 4, it also comes into contact with a corrosive PAS raw material such as an alkali metal hydroxide. By forming the valve 5 from a zirconium-containing material, not only corrosion due to hydrogen sulfide but also corrosion due to an alkali metal hydroxide can be effectively prevented.

Furthermore, the polymerization reaction of PAS is generally performed under a high temperature condition of 200 ° C. or higher. Since the valve 5 of the present embodiment is formed from a zirconium-containing material, corrosion of the valve 5 can be effectively suppressed even under high temperature conditions.

The zirconium-containing material is not particularly limited as long as zirconium is contained, and examples thereof include a metal material containing zirconium. The zirconium content in the zirconium-containing material is not particularly limited, and is preferably 95 to 100% by mass, more preferably 97.5 to 99.5% by mass from the viewpoint of improving corrosion resistance. Even more preferably, it is 98 to 99% by mass.

Hereinafter, the present invention will be described more specifically with reference to examples and comparative examples. The present invention is not limited to the examples.

[Metal sample]
The following metal samples were used.
Zirconium-containing material Inconel 600 having plasticity shown in Table 1
SUS304
SUS316L
nickel

However, the total content of Hf is 1%

[Corrosion test 1]
A metal sample having dimensions of 30 mm × 50 mm × 2 mm was immersed in a 64% by mass aqueous sodium hydrosulfide solution and allowed to stand at a temperature of 80 ° C. for 16 days, and then the degree of corrosion of the metal sample was visually observed. The result of arranging the metal samples in descending order is shown below.
SUS316L>SUS304> Inconel 600> Zirconium-containing material

[Corrosion test 2]
A metal sample having dimensions of 25 mm × 50 mm × 2 mm was placed in a 2% by mass hydrogen sulfide atmosphere (no water vapor, the balance: carbon dioxide) and allowed to stand at a pressure of 3 MPa and a temperature of 250 ° C. for 10 days. It was observed visually. The result of arranging the metal samples in descending order is shown below.
Nickel >> Inconel 600>SUS316L>Titanium> Zirconium-containing material

[Corrosion test 3]
A metal sample having a size of 25 mm × 50 mm × 2 mm was placed in a 2% by mass hydrogen sulfide atmosphere (with water vapor: RH_%, the balance: carbon dioxide), and allowed to stand at a pressure of 3.7 MPa and a temperature of 250 ° C. for 10 days. The degree of corrosion was visually observed. The result of arranging the metal samples in descending order is shown below.
Nickel >> Inconel 600 >>SUS316L>Titanium> Zirconium-containing material

[Corrosion test 4]
A metal sample, which is a sphere having a diameter of 75 mm, was immersed in a 75% by mass aqueous sodium hydroxide solution and allowed to stand at a temperature of 130 ° C. for half a year. The results of arranging the metal samples in descending order of decrease in roundness are shown below.
Inconel 600> Zirconium-containing material

From the above, the zirconium-containing material showed excellent corrosion resistance to any of the sodium hydrosulfide aqueous solution, the hydrogen sulfide atmosphere, and the sodium hydroxide aqueous solution. Therefore, in the PAS manufacturing apparatus, the corrosion resistance of the valve can be improved by forming the valve provided in the supply path for supplying the sulfur source as the raw material to the reaction tank with the zirconium-containing material.

DESCRIPTION OF SYMBOLS 1 Reaction tank 11 Cylindrical trunk | drum 12 Cover part 13 Bottom part 131 Discharge pipe 21 Stirring blade 22 Stirring shaft 3 Baffle 4 Supply path 5 Valve 100 PAS manufacturing apparatus

Claims

A reaction vessel for producing a polyarylene sulfide by polymerizing a sulfur source and a dihaloaromatic compound in an organic polar solvent;
A supply path communicating with the reaction tank and supplying the sulfur source to the reaction tank;
At least one valve provided in the supply path for opening and closing the supply path;
An apparatus for producing polyarylene sulfide comprising:
A manufacturing apparatus in which at least one of the valves is formed of a zirconium-containing material.
The manufacturing apparatus according to claim 1, wherein, among the at least one valve, a valve closest to the reaction vessel is formed from the zirconium-containing material.
The production apparatus according to claim 1 or 2, wherein the zirconium content in the zirconium-containing material is 95 to 100% by mass.