WO2018123233A1 - Method for producing vinyl chloride resin that prevents scaling - Google Patents
Method for producing vinyl chloride resin that prevents scaling Download PDFInfo
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- WO2018123233A1 WO2018123233A1 PCT/JP2017/038244 JP2017038244W WO2018123233A1 WO 2018123233 A1 WO2018123233 A1 WO 2018123233A1 JP 2017038244 W JP2017038244 W JP 2017038244W WO 2018123233 A1 WO2018123233 A1 WO 2018123233A1
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- vinyl chloride
- piping
- connection pipe
- scale
- pipe
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F14/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F14/02—Monomers containing chlorine
- C08F14/04—Monomers containing two carbon atoms
- C08F14/06—Vinyl chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/002—Scale prevention in a polymerisation reactor or its auxiliary parts
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/18—Suspension polymerisation
Definitions
- the present invention relates to a method for preventing a scale from being formed inside a connection pipe connected to an upper portion of a polymerization reactor in the production of a vinyl chloride resin.
- JP-A-56-122810 Japanese Patent Laid-Open No. 55-62908 JP-A-8-176209
- the present invention solves the problem that a scale is formed inside a connection pipe connected to the upper part of a polymerization reactor in the production of a vinyl chloride resin, and improves productivity, safety, and working environment. With the goal.
- the vacuum pump connection pipe, the safety valve connection pipe, and the foam level meter connection pipe are integrated into one connection pipe.
- a nitrogen pipe is attached to each of the connection pipe and the cleaning water / steam / vinyl chloride monomer gas recovery connection pipe. Even if the vacuum pump connection pipe, the safety valve connection pipe, and the foam level meter connection pipe are not aggregated, it is possible to respond by attaching nitrogen pipes to all connection pipes. And after completion
- the formation of scale can be prevented by sealing nitrogen into each connection pipe at the top of the polymerization reactor, thereby improving productivity, safety, and working environment. Also, by consolidating the vacuum pump connection piping, safety valve connection piping, and bubble level meter connection piping, the inspection locations can be consolidated, so the nitrogen filling locations can be consolidated, the operation can be simplified, and workability during dismantling inspection Is reduced.
- connection piping structure of the conventional polymerization reactor upper part As an example of the present invention, it is a structure in the case where the connection piping at the top of the polymerization reactor is aggregated and the nitrogen piping is connected to the connection piping. It is a photograph (safety valve 12 is removed and photographed) inside the safety valve connection pipe 12 in a comparative example. It is a photograph inside the vacuum pump connection pipe 17 in the comparative example (photographing with the horizontal flange of the connection pipe 17 removed). It is the photograph inside the bubble level meter connection piping 18 in a comparative example (photograph with the bubble level meter removed 18 ').
- Photo of cleaning water / steam / vinyl chloride monomer gas recovery connection pipe 16 in the comparative example is there. It is the photograph inside the aggregation connection piping 20 in an Example (The horizontal part flange of the aggregation connection piping 20 is removed, and imaging
- the present invention includes the following items.
- Item 1 A method for producing a vinyl chloride resin in which a nitrogen pipe is connected to a connection pipe installed in a polymerization reactor, and polymerization is performed while filling the connection pipe with nitrogen.
- Item 2 The vinyl chloride system according to item 1, wherein water, a vinyl chloride monomer, and a polymerization initiator are charged in a polymerization reactor, and after the temperature is raised to the reaction temperature, the connection pipe is filled with nitrogen in a volume equal to or greater than the volume in the connection pipe. Manufacturing method of resin.
- Item 3. The method for producing a vinyl chloride resin according to Item 1 or 2, wherein the connection piping is at least one selected from a preparation piping and an extraction piping.
- Item 4. The method for producing a vinyl chloride resin according to any one of Items 1 to 3, wherein the connection pipe is for connection of at least one selected from a safety valve, a vacuum pump, and a level meter.
- Item 5 The method for producing a vinyl chloride resin according to any one of Items 1 to 4, wherein a polymerization reactor equipped with one connection pipe is used for connection of a safety valve, a vacuum pump, and a level meter.
- a polymerization reactor connection piping scale countermeasure facility according to an embodiment of the present invention and a manufacturing method using this facility will be described in detail.
- a safety valve connection pipe 12 in addition to the reflux condenser 6, a safety valve connection pipe 12, a washing water / steam / vinyl chloride monomer gas recovery connection pipe 16, a vacuum pump connection pipe 17, a vinyl chloride monomer charging pipe 11, A polymerization initiator charging pipe 10 and a foam level meter connection pipe 18 are installed. Further, a polymerization terminator introduction pipe 19 is connected to the vacuum pump connection pipe 17.
- non-scale agent spraying device 3 and the non-scale agent spray nozzle 5 are installed through the cleaning water / steam / vinyl chloride monomer gas recovery connection pipe 16.
- the sprinkler 4 is for uniformly washing the inside of the polymerization vessel by dispersing the washing water from the washing water pipe 15 in the polymerization reactor.
- Suspension polymerization in vinyl chloride resin production is performed by a batch method.
- the polymerization reactor is provided with a jacket through which cooling water can pass and a reflux condenser 6.
- a non-scale agent coating process is started in the polymerization reactor and the reflux condenser 6.
- a non-scale agent supply tube 1 and a steam supply tube 2 are connected to the non-scale agent injection nozzle 5, and the non-scale agent and steam are mixed and injected from the non-scale agent injection nozzle 5 in the polymerization reactor and A non-scale agent is applied to the reflux condenser 6.
- pure water and a dispersant are charged from the connection pipe at the bottom of the polymerizer.
- the polymerization initiator is supplied from the polymerization initiator supply pipe 10
- the vinyl chloride monomer is supplied from the vinyl chloride monomer supply pipe 11.
- warm pure water is charged from the polymerization reactor bottom portion connecting pipe during or after the vinyl chloride monomer is charged.
- the temperature of the warm pure water is a temperature calculated so that the temperature in the polymerization reactor reaches the reaction temperature after completion of the warm pure water preparation. Thereafter, the polymerization reaction starts, and the reaction heat generated by the reaction is allowed to react while gradually heating until the heat of reaction disappears by jacket cooling and a reflux condenser.
- the reflux condenser 6 adjusts the amount of heat removal by the cooling water 7 and 8 flowing during the reaction, and the reflux condenser 6 adjusts the amount of heat removal by the total area (heat transfer area) where the vinyl chloride monomer contacts the reflux condenser tube. This is because the portion not gradually heated is filled with nitrogen, and the water is washed from the washing pipe 9 connected to the upper part of the reflux condenser when each batch slurry is taken out. Moreover, since the vinyl chloride monomer preparation piping 11 is washed with the vinyl chloride monomer in the batch vinyl chloride monomer preparation step, no scale is formed. Also for the polymerization initiator charging pipe 10, pure water is poured into the pipe until the reaction is completed after the initiator is charged, and scale is hardly formed.
- the safety valve connection pipe 12, the vacuum pump connection pipe 17, and the foam level meter connection pipe 18 that are not cleaned are formed on the inner wall or the sensor unit of the foam level meter by using the adhered vinyl chloride resin particles as seeds. Is done. This scale grows and eventually leads to blockage.
- a film-like scale is formed on the inner wall even in the washing water / steam / vinyl chloride monomer gas recovery connection pipe 16 in which each batch is washed with water.
- the safety valve connection pipe 12 If the safety valve connection pipe 12 is closed, the gas release from the chamber becomes insufficient when the safety valve is activated due to an increase in pressure due to a reaction abnormality or the like, and if the pressure further increases, a dangerous situation occurs.
- the vacuum pump connection pipe 17 is also connected with a polymerization terminator pipe 19, and when the polymerization terminator is introduced due to an abnormal reaction or the like, the charged amount becomes insufficient and the reaction cannot be stopped. There is a risk. As for the formation of scale on the bubble level meter connection pipe 18, the bubble level meter will not operate normally if it grows up.
- the cleaning water / steam / vinyl chloride monomer gas recovery connection pipe 16 is unlikely to be blocked, but it is a film-like scale that is formed on and adhered to the inner wall by washing the container with cleaning water or recovering the vinyl chloride monomer gas. Since the part peels off and gets caught by the water sprinkler 4, the in-vessel water washing after slurry removal becomes insufficient, and the residual vinyl chloride resin particles undergo additional polymerization in the reaction process of the next batch, resulting in a worse fish eye, quality. Adversely affects.
- the polymerization reactor is periodically opened to dismantle the cleaning water / steam / vinyl chloride monomer gas recovery connection pipe 16, the safety valve connection pipe 12, the vacuum pump connection pipe 17, the foam level meter connection pipe 18, and the like. Therefore, it is necessary to perform an operation for removing the attached scale, which requires a considerable amount of man-hours and time. It also affects productivity. Further, harmful vinyl chloride monomer gas is released out of the system, which is not preferable in terms of the working environment.
- FIG. 2 shows an example in which the connection pipes at the top of the polymerization reactor according to the present invention are consolidated and the nitrogen pipes are connected to the connection pipes.
- the vacuum pump connection pipe 17, the safety valve connection pipe 12, the foam level meter connection pipe 18, and the polymerization terminator introduction pipe 19 are integrated into one connection pipe 20.
- nitrogen pipes 21 and 22 were attached to the connecting pipe and the cleaning water / steam / vinyl chloride monomer gas recovery connecting pipe, respectively.
- the vacuum pump connection pipe 17, the safety valve connection pipe 12, and the bubble level meter connection pipe 18 are not consolidated, it is preferable to attach a nitrogen pipe to each connection pipe.
- the nitrogen piping valve attached to these connection pipes is opened, and nitrogen corresponding to the pipe volume or more is sealed.
- the nitrogen pressure is preferably equal to or higher than the reaction pressure.
- an accumulator in the nitrogen pipe is preferably performed every batch.
- connection pipe Care must be taken when enclosing nitrogen in the connection pipe. If the connection pipe is relatively short (approximately 50 cm or less), even if nitrogen for the volume of the connection pipe is sealed, the vinyl chloride monomer is connected by the convection. In some cases, a scale is formed in the connection pipe as a result. In this case, it is preferable to inject nitrogen intermittently or continuously after filling the pipe volume with nitrogen. The determination may be made according to the actual scale adhesion.
- FIG. 1 As a conventional method, the structure shown in FIG. 1 was used. When a copper tube is wrapped around the vacuum pump connection pipe 17, safety valve connection pipe 12, foam level meter connection pipe 18, etc. at the top of the polymerization reactor and hot water of 80 to 90 ° C. is passed through, each pipe after 100 batch continuous operation As for the internal state, scale formation was observed as shown in the internal photograph of the safety valve connection pipe 12 in FIG. 3, the internal photograph of the vacuum pump connection pipe 17 in FIG. 4, and the internal photograph of the foam level meter connection pipe 18 in FIG. Moreover, as shown in FIG. 6, the film-like scale adheres to the wall surface of the cleaning water / steam / vinyl chloride monomer gas recovery connection pipe, which cannot wind the copper tube and cannot be kept warm or cooled. The scale or the part which can be estimated that the scale has peeled off is seen.
- the present invention it is possible to modify the equipment at a low cost, and in order to exclude the reactant gas that causes the scale from the inert gas such as nitrogen, the weight is higher than the reaction gas. Since it can enclose a light inert gas, it is possible to reliably prevent the formation of scale in the upper connection piping, and it can be applied to a polymerization reactor for producing a vinyl chloride resin. Expected.
- Non-scale agent piping 2 ....
- Steam (spraying) piping 3 ....
- Non-scale agent spraying shaft 4 ....
- Sprinkler panel 5 ....
- ⁇ ⁇ ⁇ Reflux condenser 7,8 ⁇ ⁇ Reflux condenser cooling water piping 9 ⁇ ⁇ ⁇ ⁇ Reflux condenser upper washing water piping 10 ⁇ ⁇ ⁇ Polymerization initiator feeding piping 11 ⁇ ⁇ ⁇ Vinyl chloride monomer feeding piping 12 ⁇ ⁇ ⁇ Safety valve connection Piping 12 '... Safety valve 13 ... Vinyl chloride monomer gas recovery piping 14 ... Steam piping 15 ... Cleaning water piping in polymerization reactor 16 ...
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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)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
Abstract
Scale forms inside piping that connects polymerization reactors for producing vinyl chloride resins. As scale growth increases, the interior of the piping becomes blocked, hindering the polymerization process. Reaction control is particularly difficult if the safety valve connection piping is blocked. Therefore, it is necessary to disassemble the connection piping and clean the interior thereof at regular intervals. Moreover, in such instances, there is a possibility that vinyl chloride monomer gas will escape from the system, which is undesirable. Provided is a method of production with which a countermeasure for preventing such events is performed. The connection piping in the upper portion of the polymerization reactor is consolidated, and nitrogen piping 21 is joined to the connection piping 20 and filled with an amount of nitrogen corresponding to the piping volume. It is thereby possible to cause vinyl chloride monomer gas, which is the substance that causes scale to form, to be forced back from the connection piping 20 into the polymerization reactor.
Description
本発明は、塩化ビニール系樹脂の製造に際し、重合反応器上部に接続している接続配管の内部で、スケールが形成されないようにする方法に関するものである。
The present invention relates to a method for preventing a scale from being formed inside a connection pipe connected to an upper portion of a polymerization reactor in the production of a vinyl chloride resin.
塩化ビニール系樹脂の製造において、従来のスケール対策としては、重合反応器上部接続配管に銅チューブを巻くか、または２重管にして８０～９０℃の温水を通すことにより、スケール形成の元となる塩化ビニールモノマーガスを凝縮しないようにすることで、スケール形成を防止している。または対照的に、５℃前後の冷却水を通して、冷却効果による塩化ビニールモノマーガスの反応抑制によって、スケール形成を防止する方法もある。
しかし、これらの方法では、完全にはスケール形成を防止することはできず、長期におけるスケール対策には、不十分であった。 In the production of vinyl chloride resin, conventional scale countermeasures include the use of a copper tube around the upper connection pipe of the polymerization reactor, or a double pipe to pass hot water of 80 to 90 ° C, thereby reducing the scale formation. By preventing the vinyl chloride monomer gas from condensing, scale formation is prevented. Or, in contrast, there is a method of preventing scale formation by suppressing the reaction of the vinyl chloride monomer gas due to the cooling effect through cooling water at around 5 ° C.
However, these methods cannot completely prevent scale formation, and are insufficient for long-term scale countermeasures.
しかし、これらの方法では、完全にはスケール形成を防止することはできず、長期におけるスケール対策には、不十分であった。 In the production of vinyl chloride resin, conventional scale countermeasures include the use of a copper tube around the upper connection pipe of the polymerization reactor, or a double pipe to pass hot water of 80 to 90 ° C, thereby reducing the scale formation. By preventing the vinyl chloride monomer gas from condensing, scale formation is prevented. Or, in contrast, there is a method of preventing scale formation by suppressing the reaction of the vinyl chloride monomer gas due to the cooling effect through cooling water at around 5 ° C.
However, these methods cannot completely prevent scale formation, and are insufficient for long-term scale countermeasures.
本発明は、塩化ビニール系樹脂の製造に際し、重合反応器上部に接続している接続配管の内部でスケールが形成されるという課題を解決し、生産性、安全性、および作業環境を向上させることを目的とする。
The present invention solves the problem that a scale is formed inside a connection pipe connected to the upper part of a polymerization reactor in the production of a vinyl chloride resin, and improves productivity, safety, and working environment. With the goal.
本発明は、真空ポンプ接続配管、安全弁接続配管、および泡レベル計接続配管を集約して、１つの接続配管にすることが好ましい。そして、この接続配管と、洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管にそれぞれ窒素配管を付設する。真空ポンプ接続配管、安全弁接続配管、および泡レベル計接続配管を集約しなくても、全ての接続配管に窒素配管を付設することでも、対応できる。
そして、重合工程の温純水仕込み終了後に、これらの接続配管に、付設した窒素配管のバルブを開放し、配管内の容積分の窒素を封入する。 In the present invention, it is preferable that the vacuum pump connection pipe, the safety valve connection pipe, and the foam level meter connection pipe are integrated into one connection pipe. A nitrogen pipe is attached to each of the connection pipe and the cleaning water / steam / vinyl chloride monomer gas recovery connection pipe. Even if the vacuum pump connection pipe, the safety valve connection pipe, and the foam level meter connection pipe are not aggregated, it is possible to respond by attaching nitrogen pipes to all connection pipes.
And after completion | finish of warm pure water preparation of a superposition | polymerization process, the valve | bulb of nitrogen piping attached to these connection piping is open | released, and nitrogen for the volume in piping is enclosed.
そして、重合工程の温純水仕込み終了後に、これらの接続配管に、付設した窒素配管のバルブを開放し、配管内の容積分の窒素を封入する。 In the present invention, it is preferable that the vacuum pump connection pipe, the safety valve connection pipe, and the foam level meter connection pipe are integrated into one connection pipe. A nitrogen pipe is attached to each of the connection pipe and the cleaning water / steam / vinyl chloride monomer gas recovery connection pipe. Even if the vacuum pump connection pipe, the safety valve connection pipe, and the foam level meter connection pipe are not aggregated, it is possible to respond by attaching nitrogen pipes to all connection pipes.
And after completion | finish of warm pure water preparation of a superposition | polymerization process, the valve | bulb of nitrogen piping attached to these connection piping is open | released, and nitrogen for the volume in piping is enclosed.
本発明によれば、重合反応器上部の各接続配管に窒素を封入したことにより、スケールの形成を防止することができ、それにより生産性、安全性、および作業環境を向上することができる。
また、真空ポンプ接続配管、安全弁接続配管、および泡レベル計接続配管を集約することにより、点検箇所が集約できるため、窒素封入箇所が集約でき、操作が簡素化できることと、解体点検時の作業性が軽減される。 According to the present invention, the formation of scale can be prevented by sealing nitrogen into each connection pipe at the top of the polymerization reactor, thereby improving productivity, safety, and working environment.
Also, by consolidating the vacuum pump connection piping, safety valve connection piping, and bubble level meter connection piping, the inspection locations can be consolidated, so the nitrogen filling locations can be consolidated, the operation can be simplified, and workability during dismantling inspection Is reduced.
また、真空ポンプ接続配管、安全弁接続配管、および泡レベル計接続配管を集約することにより、点検箇所が集約できるため、窒素封入箇所が集約でき、操作が簡素化できることと、解体点検時の作業性が軽減される。 According to the present invention, the formation of scale can be prevented by sealing nitrogen into each connection pipe at the top of the polymerization reactor, thereby improving productivity, safety, and working environment.
Also, by consolidating the vacuum pump connection piping, safety valve connection piping, and bubble level meter connection piping, the inspection locations can be consolidated, so the nitrogen filling locations can be consolidated, the operation can be simplified, and workability during dismantling inspection Is reduced.
本発明は、下記の項などである。
項１． 重合反応器に設置する接続配管に、窒素配管を接続しておき、接続配管内を窒素で満たしながら、重合させる塩化ビニール系樹脂の製造方法。 The present invention includes the following items.
Item 1. A method for producing a vinyl chloride resin in which a nitrogen pipe is connected to a connection pipe installed in a polymerization reactor, and polymerization is performed while filling the connection pipe with nitrogen.
項１． 重合反応器に設置する接続配管に、窒素配管を接続しておき、接続配管内を窒素で満たしながら、重合させる塩化ビニール系樹脂の製造方法。 The present invention includes the following items.
項２． 重合反応器に、水、塩化ビニールモノマー、および重合開始剤を仕込み、反応温度まで昇温後、接続配管に、接続配管内の容積分以上の窒素を封入させる、項１に記載の塩化ビニール系樹脂の製造方法。
Item 2. Item 2. The vinyl chloride system according to item 1, wherein water, a vinyl chloride monomer, and a polymerization initiator are charged in a polymerization reactor, and after the temperature is raised to the reaction temperature, the connection pipe is filled with nitrogen in a volume equal to or greater than the volume in the connection pipe. Manufacturing method of resin.
項３． 接続配管が、仕込み配管および抜き出し配管から選択された少なくとも１つである、項１または項２に記載の塩化ビニール系樹脂の製造方法。
Item 3. Item 3. The method for producing a vinyl chloride resin according to Item 1 or 2, wherein the connection piping is at least one selected from a preparation piping and an extraction piping.
項４． 接続配管が、安全弁、真空ポンプ、およびレベル計から選択された少なくとも１つの接続用である、項１から項３のいずれか１項に記載の塩化ビニール系樹脂の製造方法。
Item 4. Item 4. The method for producing a vinyl chloride resin according to any one of Items 1 to 3, wherein the connection pipe is for connection of at least one selected from a safety valve, a vacuum pump, and a level meter.
項５． 安全弁、真空ポンプ、およびレベル計の接続用として、１つの接続配管を設置した重合反応器を用いる、項１から項４のいずれか１項に記載の塩化ビニール系樹脂の製造方法
Item 5. Item 5. The method for producing a vinyl chloride resin according to any one of Items 1 to 4, wherein a polymerization reactor equipped with one connection pipe is used for connection of a safety valve, a vacuum pump, and a level meter.
以下、図面を適宜参照して、本発明の実施形態における重合反応器接続配管スケール対策設備、およびこの設備を用いた製造方法について、詳細に説明する。
図１の通り、重合反応器上部には、還流コンデンサー６以外に、安全弁接続配管１２、洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管１６、真空ポンプ接続配管１７、塩化ビニールモノマー仕込み配管１１、重合開始剤仕込み配管１０、および泡レベル計接続配管１８を設置している。また、真空ポンプ接続配管１７には、重合停止剤投入配管１９を接続している。 Hereinafter, with reference to the drawings as appropriate, a polymerization reactor connection piping scale countermeasure facility according to an embodiment of the present invention and a manufacturing method using this facility will be described in detail.
As shown in FIG. 1, in addition to thereflux condenser 6, a safety valve connection pipe 12, a washing water / steam / vinyl chloride monomer gas recovery connection pipe 16, a vacuum pump connection pipe 17, a vinyl chloride monomer charging pipe 11, A polymerization initiator charging pipe 10 and a foam level meter connection pipe 18 are installed. Further, a polymerization terminator introduction pipe 19 is connected to the vacuum pump connection pipe 17.
図１の通り、重合反応器上部には、還流コンデンサー６以外に、安全弁接続配管１２、洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管１６、真空ポンプ接続配管１７、塩化ビニールモノマー仕込み配管１１、重合開始剤仕込み配管１０、および泡レベル計接続配管１８を設置している。また、真空ポンプ接続配管１７には、重合停止剤投入配管１９を接続している。 Hereinafter, with reference to the drawings as appropriate, a polymerization reactor connection piping scale countermeasure facility according to an embodiment of the present invention and a manufacturing method using this facility will be described in detail.
As shown in FIG. 1, in addition to the
また、洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管１６の内部を通して、ノンスケール剤噴霧装置３およびノンスケール剤噴霧ノズル５が設置されている。散水盤４は、重合反応器内洗浄水配管１５からの洗浄水を分散させて、重合器内全体を満遍なく洗浄するためのものである。
Further, the non-scale agent spraying device 3 and the non-scale agent spray nozzle 5 are installed through the cleaning water / steam / vinyl chloride monomer gas recovery connection pipe 16. The sprinkler 4 is for uniformly washing the inside of the polymerization vessel by dispersing the washing water from the washing water pipe 15 in the polymerization reactor.
塩化ビニール系樹脂製造における懸濁重合は、バッチ方式により行われている。重合反応器は冷却水を通すことができるジャケットと還流コンデンサー６が付設されている。この重合工程では、まず重合反応器内および還流コンデンサー６へのノンスケール剤塗布工程からスタートする。ノンスケール剤噴射ノズル５にノンスケール剤供給チューブ１とスチーム供給チューブ２が接続されており、ノンスケール剤とスチームを混合してノンスケール剤噴射ノズル５からこれらを噴射し、重合反応器内および還流コンデンサー６へノンスケール剤を塗布する。
Suspension polymerization in vinyl chloride resin production is performed by a batch method. The polymerization reactor is provided with a jacket through which cooling water can pass and a reflux condenser 6. In this polymerization process, first, a non-scale agent coating process is started in the polymerization reactor and the reflux condenser 6. A non-scale agent supply tube 1 and a steam supply tube 2 are connected to the non-scale agent injection nozzle 5, and the non-scale agent and steam are mixed and injected from the non-scale agent injection nozzle 5 in the polymerization reactor and A non-scale agent is applied to the reflux condenser 6.
次に、重合反応器開放後であれば器内を脱酸素目的で真空ポンプ接続配管１７を通して真空にする工程が行われ、その後水仕込みが行われる。重合反応器は密閉のまま連続スタートするのであれば、真空工程は行われず、水仕込みがスタートする。
Next, if the polymerization reactor is opened, a process of evacuating the inside of the reactor through the vacuum pump connection pipe 17 for the purpose of deoxidation is performed, and then water is charged. If the polymerization reactor is continuously started in a sealed state, the vacuum process is not performed and the water charging starts.
水仕込みでは、純水および分散剤が、重合器ボトム部接続配管から仕込まれる。水仕込み終了後、重合開始剤が重合開始剤仕込み配管１０より仕込まれ、そして塩化ビニールモノマー仕込み配管１１から塩化ビニールモノマーが仕込まれる。また、塩化ビニールモノマー仕込み中、または仕込み終了後に、重合器ボトム部接続配管から温純水が仕込まれる。温純水の温度は、温純水仕込み終了後に、重合反応器内が反応温度に到達するよう演算された温度となっている。その後、重合反応が始まり、反応により発生する反応熱をジャケット冷却と還流コンデンサーにより反応熱がなくなるまで徐熱しながら反応させる。
In the water charge, pure water and a dispersant are charged from the connection pipe at the bottom of the polymerizer. After the completion of the water preparation, the polymerization initiator is supplied from the polymerization initiator supply pipe 10, and the vinyl chloride monomer is supplied from the vinyl chloride monomer supply pipe 11. Also, warm pure water is charged from the polymerization reactor bottom portion connecting pipe during or after the vinyl chloride monomer is charged. The temperature of the warm pure water is a temperature calculated so that the temperature in the polymerization reactor reaches the reaction temperature after completion of the warm pure water preparation. Thereafter, the polymerization reaction starts, and the reaction heat generated by the reaction is allowed to react while gradually heating until the heat of reaction disappears by jacket cooling and a reflux condenser.
各箇所のスケール形成に関して、まず還流コンデンサー６内部はスケールがほとんど形成されることはない。それは、還流コンデンサー６は反応中に冷却水７および８が流れていること、還流コンデンサー６は塩化ビニールモノマーが還流コンデンサー内チューブに接触させる総面積（伝熱面積）によって除熱量を調節しており徐熱していない部分は窒素が封入されていること、そして毎バッチスラリー抜出時に還流コンデンサー上部に接続された洗浄配管９より水洗が行われるからである。また、塩化ビニールモノマー仕込み配管１１は、毎バッチ塩化ビニールモノマー仕込み工程で塩化ビニールモノマーによって洗浄されているため、スケールが形成されない。重合開始剤仕込み配管１０についても、開始剤仕込み後反応が終了するまで配管内に純水を注水しており、スケールが形成されることはほとんどない。
Regarding the scale formation at each location, first, almost no scale is formed inside the reflux condenser 6. The reflux condenser 6 adjusts the amount of heat removal by the cooling water 7 and 8 flowing during the reaction, and the reflux condenser 6 adjusts the amount of heat removal by the total area (heat transfer area) where the vinyl chloride monomer contacts the reflux condenser tube. This is because the portion not gradually heated is filled with nitrogen, and the water is washed from the washing pipe 9 connected to the upper part of the reflux condenser when each batch slurry is taken out. Moreover, since the vinyl chloride monomer preparation piping 11 is washed with the vinyl chloride monomer in the batch vinyl chloride monomer preparation step, no scale is formed. Also for the polymerization initiator charging pipe 10, pure water is poured into the pipe until the reaction is completed after the initiator is charged, and scale is hardly formed.
しかし、洗浄がされない安全弁接続配管１２、真空ポンプ接続配管１７、および泡レベル計接続配管１８は、付着した塩化ビニール系樹脂の粒子を種にして、内壁または泡レベル計のセンサー部にスケールが形成される。このスケールは、次第に成長し、やがては閉塞に繋がっていく。
However, the safety valve connection pipe 12, the vacuum pump connection pipe 17, and the foam level meter connection pipe 18 that are not cleaned are formed on the inner wall or the sensor unit of the foam level meter by using the adhered vinyl chloride resin particles as seeds. Is done. This scale grows and eventually leads to blockage.
また、毎バッチ水洗が行われている洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管１６でも、内壁にフィルム状のスケールが形成される。安全弁接続配管１２が閉塞すると、反応異常等による圧力上昇での安全弁作動時に器内ガス放出が不十分となり、圧力が更に上昇すれば危険な事態に陥る。また、真空ポンプ接続配管１７についても、この配管に重合停止剤配管１９が接続されており、異常反応等で重合停止剤を投入したときに投入量が不十分となり、反応を止めることができなくなる危険性がある。泡レベル計接続配管１８へのスケール形成についても、成長すれば泡レベル計が正常に作動しなくなる。洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管１６は閉塞にまで至ることは少ないが、洗浄水による器内水洗や塩化ビニールモノマーガス回収等によって、内壁に形成、付着したフィルム状のスケールの一部が剥がれ落ち、散水盤４に引っかかるため、スラリー抜出後の器内水洗が不十分となり、残留した塩化ビニール系樹脂粒子が次バッチの反応工程で追加重合し、フィッシュアイが悪化し、品質に悪影響を与える。
In addition, a film-like scale is formed on the inner wall even in the washing water / steam / vinyl chloride monomer gas recovery connection pipe 16 in which each batch is washed with water. If the safety valve connection pipe 12 is closed, the gas release from the chamber becomes insufficient when the safety valve is activated due to an increase in pressure due to a reaction abnormality or the like, and if the pressure further increases, a dangerous situation occurs. The vacuum pump connection pipe 17 is also connected with a polymerization terminator pipe 19, and when the polymerization terminator is introduced due to an abnormal reaction or the like, the charged amount becomes insufficient and the reaction cannot be stopped. There is a risk. As for the formation of scale on the bubble level meter connection pipe 18, the bubble level meter will not operate normally if it grows up. The cleaning water / steam / vinyl chloride monomer gas recovery connection pipe 16 is unlikely to be blocked, but it is a film-like scale that is formed on and adhered to the inner wall by washing the container with cleaning water or recovering the vinyl chloride monomer gas. Since the part peels off and gets caught by the water sprinkler 4, the in-vessel water washing after slurry removal becomes insufficient, and the residual vinyl chloride resin particles undergo additional polymerization in the reaction process of the next batch, resulting in a worse fish eye, quality. Adversely affects.
このために、定期的に重合反応器を開放して洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管１６、安全弁接続配管１２、真空ポンプ接続配管１７、泡レベル計接続配管１８などを解体して、付着したスケールを取り除く作業を行わなければならず、かなりの工数と時間を要する。生産性にも影響する。また、有害な塩化ビニールモノマーガスを系外に放出することになり、作業環境上好ましくない。
For this purpose, the polymerization reactor is periodically opened to dismantle the cleaning water / steam / vinyl chloride monomer gas recovery connection pipe 16, the safety valve connection pipe 12, the vacuum pump connection pipe 17, the foam level meter connection pipe 18, and the like. Therefore, it is necessary to perform an operation for removing the attached scale, which requires a considerable amount of man-hours and time. It also affects productivity. Further, harmful vinyl chloride monomer gas is released out of the system, which is not preferable in terms of the working environment.
以下、図２について、図１からの相違点について、説明を行う。
図２は、本発明による重合反応器上部の接続配管の集約、接続配管への窒素配管接続を行なった実施例である。真空ポンプ接続配管１７、安全弁接続配管１２、泡レベル計接続配管１８、および重合停止剤投入配管１９を、集約して、１つの接続配管２０とした。そして、この接続配管と、洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管にそれぞれ窒素配管２１および２２を付設した。
真空ポンプ接続配管１７、安全弁接続配管１２、および泡レベル計接続配管１８を集約しない場合は、それぞれの接続配管に窒素配管を付設することが好ましい。 Hereinafter, the differences from FIG. 1 will be described with reference to FIG.
FIG. 2 shows an example in which the connection pipes at the top of the polymerization reactor according to the present invention are consolidated and the nitrogen pipes are connected to the connection pipes. The vacuumpump connection pipe 17, the safety valve connection pipe 12, the foam level meter connection pipe 18, and the polymerization terminator introduction pipe 19 are integrated into one connection pipe 20. Then, nitrogen pipes 21 and 22 were attached to the connecting pipe and the cleaning water / steam / vinyl chloride monomer gas recovery connecting pipe, respectively.
When the vacuumpump connection pipe 17, the safety valve connection pipe 12, and the bubble level meter connection pipe 18 are not consolidated, it is preferable to attach a nitrogen pipe to each connection pipe.
図２は、本発明による重合反応器上部の接続配管の集約、接続配管への窒素配管接続を行なった実施例である。真空ポンプ接続配管１７、安全弁接続配管１２、泡レベル計接続配管１８、および重合停止剤投入配管１９を、集約して、１つの接続配管２０とした。そして、この接続配管と、洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管にそれぞれ窒素配管２１および２２を付設した。
真空ポンプ接続配管１７、安全弁接続配管１２、および泡レベル計接続配管１８を集約しない場合は、それぞれの接続配管に窒素配管を付設することが好ましい。 Hereinafter, the differences from FIG. 1 will be described with reference to FIG.
FIG. 2 shows an example in which the connection pipes at the top of the polymerization reactor according to the present invention are consolidated and the nitrogen pipes are connected to the connection pipes. The vacuum
When the vacuum
重合工程の温純水仕込み終了後の反応圧力に達するタイミングで、これらの接続配管に、付設した窒素配管のバルブを開放し、配管容積分またはそれ以上の窒素を封入する。窒素の圧力は、反応圧力以上の圧力であることが好ましい。また、窒素の封入量を測るために、窒素配管に積算計を設置することが好ましい。この窒素封入工程は、毎バッチ行なうことが好ましい。
At the timing of reaching the reaction pressure after the completion of the warm pure water charging in the polymerization process, the nitrogen piping valve attached to these connection pipes is opened, and nitrogen corresponding to the pipe volume or more is sealed. The nitrogen pressure is preferably equal to or higher than the reaction pressure. In order to measure the amount of nitrogen enclosed, it is preferable to install an accumulator in the nitrogen pipe. This nitrogen sealing step is preferably performed every batch.
窒素を接続配管に封入する際に注意しなければならないことは、接続配管が比較的短い場合（おおよそ５０ｃｍ以下）、接続配管容積分の窒素を封入しても、対流によって塩化ビニールモノマーが接続配管内に混入して、その結果接続配管内にスケールを形成してしまう場合がある。この場合は、配管容積分窒素を封入後、間欠的に、または連続的に、窒素を注入することが好ましい。その判断は実際のスケールの付着状況によって、対応すればよい。
Care must be taken when enclosing nitrogen in the connection pipe. If the connection pipe is relatively short (approximately 50 cm or less), even if nitrogen for the volume of the connection pipe is sealed, the vinyl chloride monomer is connected by the convection. In some cases, a scale is formed in the connection pipe as a result. In this case, it is preferable to inject nitrogen intermittently or continuously after filling the pipe volume with nitrogen. The determination may be made according to the actual scale adhesion.
これによって重合反応器接続配管内へのスケール形成は激減し、３００バッチ連続運転後での集約配管２０の内部は、図７の通り、ほとんどスケール付着は見られなかった。また、洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管１６も同様に、スケール付着が、図８の通り、見られなかった。
The scale formation in the polymerization reactor connection pipe was drastically reduced by this, and almost no scale adhesion was observed inside the aggregated pipe 20 after 300 batch continuous operation as shown in FIG. Similarly, no scale adhesion was observed in the cleaning water / steam / vinyl chloride monomer gas recovery connection pipe 16 as shown in FIG.
（比較例）
従来の方法として、図１の構造で製造を行った。
重合反応器上部の真空ポンプ接続配管１７、安全弁接続配管１２、泡レベル計接続配管１８などに、銅チューブを巻いて８０～９０℃の温水を通した場合、１００バッチ連続運転後のそれぞれの配管の内部状況は、図３の安全弁接続配管１２内部写真、図４の真空ポンプ接続配管１７内部写真、図５の泡レベル計接続配管１８内部写真の通りのスケール形成が見られた。また、銅チューブを巻くことができず、保温または冷却ができない洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管内部は、図６の通り、壁面にフィルム状のスケールが付着し、剥がれかかっているスケール、またはスケールが剥がれていると推測できる箇所が見られる。 (Comparative example)
As a conventional method, the structure shown in FIG. 1 was used.
When a copper tube is wrapped around the vacuumpump connection pipe 17, safety valve connection pipe 12, foam level meter connection pipe 18, etc. at the top of the polymerization reactor and hot water of 80 to 90 ° C. is passed through, each pipe after 100 batch continuous operation As for the internal state, scale formation was observed as shown in the internal photograph of the safety valve connection pipe 12 in FIG. 3, the internal photograph of the vacuum pump connection pipe 17 in FIG. 4, and the internal photograph of the foam level meter connection pipe 18 in FIG. Moreover, as shown in FIG. 6, the film-like scale adheres to the wall surface of the cleaning water / steam / vinyl chloride monomer gas recovery connection pipe, which cannot wind the copper tube and cannot be kept warm or cooled. The scale or the part which can be estimated that the scale has peeled off is seen.
従来の方法として、図１の構造で製造を行った。
重合反応器上部の真空ポンプ接続配管１７、安全弁接続配管１２、泡レベル計接続配管１８などに、銅チューブを巻いて８０～９０℃の温水を通した場合、１００バッチ連続運転後のそれぞれの配管の内部状況は、図３の安全弁接続配管１２内部写真、図４の真空ポンプ接続配管１７内部写真、図５の泡レベル計接続配管１８内部写真の通りのスケール形成が見られた。また、銅チューブを巻くことができず、保温または冷却ができない洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管内部は、図６の通り、壁面にフィルム状のスケールが付着し、剥がれかかっているスケール、またはスケールが剥がれていると推測できる箇所が見られる。 (Comparative example)
As a conventional method, the structure shown in FIG. 1 was used.
When a copper tube is wrapped around the vacuum
以上のように、本発明においては、低コストでの設備改造が可能であり、窒素等の不活性ガスによってスケールの要因となる反応物ガスを系外に除外させるために、反応ガスよりも重量が軽い不活性ガスを封入しておくことができるため、上部の接続配管について、確実にスケール形成を防止することができるものであり、塩化ビニール系樹脂製造のための重合反応器に適用され得るものと、期待される。
As described above, in the present invention, it is possible to modify the equipment at a low cost, and in order to exclude the reactant gas that causes the scale from the inert gas such as nitrogen, the weight is higher than the reaction gas. Since it can enclose a light inert gas, it is possible to reliably prevent the formation of scale in the upper connection piping, and it can be applied to a polymerization reactor for producing a vinyl chloride resin. Expected.
１・・・・ノンスケール剤配管
２・・・・スチーム（噴霧用）配管
３・・・・ノンスケール剤噴霧用シャフト
４・・・・散水盤
５・・・・ノンスケール剤噴霧ノズル
６・・・・還流コンデンサー
７，８・・還流コンデンサー冷却水配管
９・・・・還流コンデンサー上部洗浄水配管
１０・・・重合開始剤仕込み配管
１１・・・塩化ビニールモノマー仕込み配管
１２・・・安全弁接続配管
１２’・・・安全弁
１３・・・塩化ビニールモノマーガス回収配管
１４・・・スチーム配管
１５・・・重合反応器内洗浄水配管
１６・・・洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管
１７・・・真空ポンプ接続配管
１７’・・・真空ポンプ
１８・・・泡レベル計接続配管
１８’・・泡レベル計
１９・・・重合停止剤投入配管
２０・・・安全弁／泡レベル計／真空ポンプ／重合停止剤投入集約接続配管
２１・・・安全弁／泡レベル計／真空ポンプ／重合停止剤投入集約接続配管用窒素配管
２２・・・洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管用窒素配管 1 .... Non-scale agent piping 2 .... Steam (spraying) piping 3 .... Non-scaleagent spraying shaft 4 .... Sprinkler panel 5 .... Non-scaling agent spray nozzle 6.・ ・ ・ Reflux condenser 7,8 ・ ・ Reflux condenser cooling water piping 9 ・ ・ ・ ・ Reflux condenser upper washing water piping 10 ・ ・ ・ Polymerization initiator feeding piping 11 ・ ・ ・ Vinyl chloride monomer feeding piping 12 ・ ・ ・ Safety valve connection Piping 12 '... Safety valve 13 ... Vinyl chloride monomer gas recovery piping 14 ... Steam piping 15 ... Cleaning water piping in polymerization reactor 16 ... Washing water / steam / vinyl chloride monomer gas recovery connection piping 17 ... Vacuum pump connection pipe 17 '... Vacuum pump 18 ... Bubble level meter connection pipe 18' ... Bubble level meter 19 ... Polymerization stopper charging pipe 20 ... Low Valve / Foam level meter / Vacuum pump / Polymerization stop agent input consolidated connection piping 21 ... Safety valve / Foam level meter / Vacuum pump / Polymerization stop agent input consolidated connection piping 22 ... Cleaning water / Vapor / Vinyl chloride Nitrogen piping for monomer gas recovery connection piping
２・・・・スチーム（噴霧用）配管
３・・・・ノンスケール剤噴霧用シャフト
４・・・・散水盤
５・・・・ノンスケール剤噴霧ノズル
６・・・・還流コンデンサー
７，８・・還流コンデンサー冷却水配管
９・・・・還流コンデンサー上部洗浄水配管
１０・・・重合開始剤仕込み配管
１１・・・塩化ビニールモノマー仕込み配管
１２・・・安全弁接続配管
１２’・・・安全弁
１３・・・塩化ビニールモノマーガス回収配管
１４・・・スチーム配管
１５・・・重合反応器内洗浄水配管
１６・・・洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管
１７・・・真空ポンプ接続配管
１７’・・・真空ポンプ
１８・・・泡レベル計接続配管
１８’・・泡レベル計
１９・・・重合停止剤投入配管
２０・・・安全弁／泡レベル計／真空ポンプ／重合停止剤投入集約接続配管
２１・・・安全弁／泡レベル計／真空ポンプ／重合停止剤投入集約接続配管用窒素配管
２２・・・洗浄水／蒸気／塩化ビニールモノマーガス回収接続配管用窒素配管 1 .... Non-scale agent piping 2 .... Steam (spraying) piping 3 .... Non-scale
Claims (5)
- 重合反応器に設置する接続配管に、窒素配管を接続しておき、接続配管内を窒素で満たしながら、重合させる塩化ビニール系樹脂の製造方法。 A method for producing a vinyl chloride resin in which a nitrogen pipe is connected to a connection pipe installed in a polymerization reactor, and polymerization is performed while filling the connection pipe with nitrogen.
- 重合反応器に、水、塩化ビニールモノマー、および重合開始剤を仕込み、反応温度まで昇温後、接続配管に、接続配管内の容積分以上の窒素を封入させる、請求項１に記載の塩化ビニール系樹脂の製造方法。 2. The vinyl chloride according to claim 1, wherein water, vinyl chloride monomer, and a polymerization initiator are charged in a polymerization reactor, and after raising the temperature to the reaction temperature, the connection pipe is filled with nitrogen in a volume equal to or greater than the volume in the connection pipe. Method for production of resin.
- 接続配管が、仕込み配管および抜き出し配管から選択された少なくとも１つである、請求項１または請求項２に記載の塩化ビニール系樹脂の製造方法。 The method for producing a vinyl chloride resin according to claim 1 or 2, wherein the connection pipe is at least one selected from a preparation pipe and an extraction pipe.
- 接続配管が、安全弁、真空ポンプ、およびレベル計から選択された少なくとも１つの接続用である、請求項１から請求項３のいずれか１項に記載の塩化ビニール系樹脂の製造方法。 The method for producing a vinyl chloride resin according to any one of claims 1 to 3, wherein the connection pipe is for connection of at least one selected from a safety valve, a vacuum pump, and a level meter.
- 安全弁、真空ポンプ、およびレベル計の接続用として、１つの接続配管を設置した重合反応器を用いる、請求項１から請求項４のいずれか１項に記載の塩化ビニール系樹脂の製造方法。 The method for producing a vinyl chloride resin according to any one of claims 1 to 4, wherein a polymerization reactor provided with one connection pipe is used for connection of a safety valve, a vacuum pump, and a level meter.
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|---|---|---|---|
| CN201780077522.3A CN110088141A (en) | 2016-12-27 | 2017-10-24 | The manufacturing method for the ethlyene dichloride system resin for preventing dirt from adhering to |
| AU2017389285A AU2017389285B2 (en) | 2016-12-27 | 2017-10-24 | Method for manufacturing vinyl chloride-based resin for preventing scale deposition |
| KR1020197012932A KR20190096951A (en) | 2016-12-27 | 2017-10-24 | Manufacturing Method of Vinyl Chloride Resin to Prevent Scale Attachment |
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| JP2016-253606 | 2016-12-27 | ||
| JP2016253606A JP2018104591A (en) | 2016-12-27 | 2016-12-27 | Manufacturing method of vinyl chloride resin for preventing scale adhesion |
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| WO2018123233A1 true WO2018123233A1 (en) | 2018-07-05 |
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| PCT/JP2017/038244 WO2018123233A1 (en) | 2016-12-27 | 2017-10-24 | Method for producing vinyl chloride resin that prevents scaling |
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| JP (1) | JP2018104591A (en) |
| KR (1) | KR20190096951A (en) |
| CN (1) | CN110088141A (en) |
| AU (1) | AU2017389285B2 (en) |
| TW (1) | TW201823274A (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114321715A (en) * | 2021-11-25 | 2022-04-12 | 青海盐湖海纳化工有限公司 | Chloroethylene storage tank water injection system |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114682182A (en) * | 2020-12-28 | 2022-07-01 | 中昊晨光化工研究院有限公司 | Device system and method for producing polymer by gas phase method |
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- 2017-10-24 WO PCT/JP2017/038244 patent/WO2018123233A1/en active Application Filing
- 2017-10-24 CN CN201780077522.3A patent/CN110088141A/en active Pending
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- 2017-10-24 KR KR1020197012932A patent/KR20190096951A/en not_active IP Right Cessation
- 2017-11-06 TW TW106138331A patent/TW201823274A/en unknown
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| JPH04170406A (en) * | 1990-11-02 | 1992-06-18 | Nippon Zeon Co Ltd | Production of vinyl chloride polymer |
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| Publication number | Publication date |
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| KR20190096951A (en) | 2019-08-20 |
| JP2018104591A (en) | 2018-07-05 |
| TW201823274A (en) | 2018-07-01 |
| AU2017389285A1 (en) | 2019-06-27 |
| CN110088141A (en) | 2019-08-02 |
| AU2017389285B2 (en) | 2022-08-04 |
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