TW202012461A - Device for residual-monomer removal - Google Patents

Device for residual-monomer removal Download PDF

Info

Publication number
TW202012461A
TW202012461A TW108118307A TW108118307A TW202012461A TW 202012461 A TW202012461 A TW 202012461A TW 108118307 A TW108118307 A TW 108118307A TW 108118307 A TW108118307 A TW 108118307A TW 202012461 A TW202012461 A TW 202012461A
Authority
TW
Taiwan
Prior art keywords
warm water
slurry
water spray
porous plate
pressure
Prior art date
Application number
TW108118307A
Other languages
Chinese (zh)
Inventor
千代田孝弘
水田浩正
佐野典久
Original Assignee
日商捷恩智股份有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 日商捷恩智股份有限公司 filed Critical 日商捷恩智股份有限公司
Publication of TW202012461A publication Critical patent/TW202012461A/en

Links

Images

Classifications

    • 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
    • C08F6/00—Post-polymerisation treatments
    • C08F6/001—Removal of residual monomers by physical means
    • 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
    • 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
    • C08F6/00—Post-polymerisation treatments
    • C08F6/24—Treatment of polymer suspensions

Landscapes

  • 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)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

A device for residual-monomer removal by which residual monomers can be efficiently removed from a slurry containing a vinyl-chloride-based resin, while preventing the residual monomers from being discharged from the process. The device for residual-monomer removal comprises: a column body 4; a plurality of perforated plates 34 disposed along the vertical direction within the column body; a plurality of chambers 16-21 formed respectively over the perforated plates serving as bottom surfaces; slurry introduction pipes 22 and 23; flow pipes 36 for causing the slurry to flow downward successively from the perforated plate beneath an upper chamber; a steam introduction pipe 10 disposed in the bottom part of the column body; a condenser 6 disposed over the upper part of the column body, with a gas discharge port 11 disposed therebetween; a slurry discharge port 24 provided to the lowermost perforated plate; and warm-water ejectors disposed just beneath the perforated plates and each including a warm-water ejection ring 38. Each warm-water ejector is provided with: a pressure gauge 40 for monitoring the ejection pressure to effectively conduct the ejection; a device for adjusting the pressure (a pressure control valve 32 or a warm-water pump 8 with inverter control); and a sight-glass-washing nozzle 37 connected to the upper part of the warm-water ejection ring 38 of the warm-water ejector or inserted into the ring.

Description

殘留單體除去裝置Residual monomer removal device

本發明是有關於一種於製造氯化乙烯系樹脂（以下，簡稱為聚氯乙烯（Polyvinyl chloride，PVC））時，可將PVC與水性介質的混合物（以下簡稱為PVC漿料）所含的以氯化乙烯單體（以下簡稱為乙烯基單體（Vinyl monomer，VCM））等為主的未反應單體進行高效地除去的、源自含氯化乙烯系樹脂漿料的未反應單體的除去裝置及除去方法。The present invention relates to a mixture of PVC and an aqueous medium (hereinafter referred to as PVC slurry) that can be included in the production of vinyl chloride-based resins (hereinafter referred to as Polyvinyl chloride (PVC)). Vinyl monomer (hereinafter abbreviated as vinyl monomer (VCM)) and other unreacted monomers that are efficiently removed and derived from unreacted monomers containing vinyl chloride-based resin slurry Removal device and removal method.

PVC是在化學性上物理性上皆具有優異的特性的樹脂，因此被使用於廣泛領域。通常，PVC是藉由懸浮聚合法、乳液聚合法、塊狀聚合法等而製造，但由於具有易於除去反應熱、而可獲得雜質少的產品的優點，而特別廣泛地應用懸浮聚合法或乳液聚合法。PVC is a resin that has excellent characteristics both chemically and physically, so it is used in a wide range of fields. Generally, PVC is manufactured by a suspension polymerization method, an emulsion polymerization method, a bulk polymerization method, etc. However, due to the advantage of easily removing the reaction heat and obtaining a product with few impurities, the suspension polymerization method or emulsion is particularly widely used Polymerization method.

懸浮聚合法或乳液聚合法，通常是藉由將VCM與水性介質、分散劑或乳化劑、及聚合起始劑等一起加入附帶攪拌機的聚合器內，一邊保持規定溫度一邊進行攪拌下使其聚合而進行。聚合反應通常並非實施至VCM100%轉化而成為PVC為止，而於製造效率良好的階段、即於聚合轉化率為80～95%的階段停止。在聚合反應結束後，聚合器內的未反應單體與PVC漿料（主要為PVC粒子與水性介質的混合分散液）分離而被回收，但於PVC漿料中通常含有幾%的未反應單體。Suspension polymerization or emulsion polymerization is usually carried out by adding VCM together with an aqueous medium, a dispersant or emulsifier, and a polymerization initiator into a polymerizer equipped with a stirrer, and stirring and polymerizing while maintaining a predetermined temperature And proceed. The polymerization reaction is usually not carried out until 100% conversion of VCM into PVC, but it is stopped at a stage where the production efficiency is good, that is, at a stage where the polymerization conversion rate is 80 to 95%. After the polymerization reaction, the unreacted monomers in the polymerizer are separated from the PVC slurry (mainly the mixed dispersion of PVC particles and aqueous medium) to be recovered, but the PVC slurry usually contains a few% of unreacted monomers body.

藉此，含有未反應單體的PVC漿料與水性介質機械地分離，藉由熱風乾燥及其他各種方法進行乾燥，而形成PVC粉末。此時，被分離的水性介質、藉由熱風乾燥所產生的廢氣、及所獲得的PVC粉末中含有因環境衛生上的理由而成為問題、或被明顯認為有害的程度的VCM。In this way, the PVC slurry containing unreacted monomers is mechanically separated from the aqueous medium, and dried by hot air drying and various other methods to form PVC powder. At this time, the separated aqueous medium, the exhaust gas generated by hot air drying, and the obtained PVC powder contain VCM to the extent that it is a problem for environmental sanitation reasons, or is clearly considered harmful.

為了將此種製造上產生的排出物及PVC粉末中的VCM完全地除去，或使其含量降低至在環境衛生上無害的程度，而提議有各種方法。例如，專利文獻1及專利文獻2例舉有使用在內部安裝有多個多孔板製擱板與在底部安裝有水蒸氣噴入口的處理塔，自PVC漿料將未反應單體除去回收的方法。In order to completely remove the effluent produced in such production and the VCM in the PVC powder, or to reduce its content to a level that is not harmful to environmental hygiene, various methods have been proposed. For example, Patent Document 1 and Patent Document 2 exemplify a method of removing unreacted monomers from PVC slurry by using a treatment tower with a plurality of perforated plate shelves installed inside and a steam injection port installed at the bottom. .

所述方法為，使用多孔板製擱板，所述多孔板製擱板的底面由多孔板構成，在所述多孔板上以形成交錯狀的處理通路的方式設置有擋板，使PVC漿料沿著所述多孔板製擱板上的處理通路順次流下，在此期間，將PVC漿料暴露於穿過多孔板的細孔而自下方噴入而來的水蒸氣中，將PVC漿料所含的未反應單體進行蒸發分離。The method is to use a shelf made of a perforated plate, the bottom surface of the shelf made of a perforated plate is composed of a perforated plate, and a baffle plate is provided on the perforated plate in a manner to form a staggered processing path to make PVC slurry Along the treatment channel on the perforated plate shelf, the PVC slurry was exposed to water vapor sprayed from below through the pores of the perforated plate during the period. The unreacted monomers contained are separated by evaporation.

通常，稱此種將未反應單體進行除去回收的方法為脫單體法，當前，所述脫單體法佔據主流。 使用所述脫單體法的未反應單體除去裝置中具有在各室的多孔板的正下方至少朝向所述多孔板的下表面而設置的溫水噴射裝置。於使PVC漿料沿著多孔板上的處理通路順次流下的期間，因系統內溫度的降低或蒸氣流量的變動等，而有漿料因室內的壓力變動而自多孔板的孔朝下方的室降下從而PVC將孔堵塞的情形，或漿料朝壁面飛散並附著的情形。若置之不理，則因多孔板的孔閉塞而水蒸氣的吹入變得不均一，因此運轉變得不穩定，從而PVC漿料中的未反應單體的除去變得不充分。又，附著於壁面的PVC因熱而變色從而作為異物污染物（Contamination）對品質帶來惡劣影響。藉由溫水噴射裝置實施的溫水噴射可沖洗附著於多孔板的孔或壁面的漿料，因此防止所述問題。Generally, this method for removing and recovering unreacted monomers is called a demonomerization method, and currently, the demonomerization method occupies the mainstream. The unreacted monomer removal device using the demonomerization method includes a warm water spray device provided directly below the porous plate of each chamber toward at least the lower surface of the porous plate. During the period in which the PVC slurry flows down along the processing path on the perforated plate sequentially, there is a room where the slurry is directed downward from the hole of the perforated plate due to the pressure change in the system due to a decrease in the temperature in the system or a change in the steam flow rate. The case where the PVC is blocked by the lowering, or the slurry is scattered and attached to the wall surface. If left unattended, the pores of the perforated plate are blocked and the blowing of water vapor becomes uneven, so the operation becomes unstable, and the removal of unreacted monomers in the PVC slurry becomes insufficient. In addition, the PVC attached to the wall surface is discolored due to heat, which has a bad influence on the quality as a foreign matter contamination. The warm water spraying by the warm water spraying device can wash the slurry adhering to the holes or the wall surface of the porous plate, thus preventing the problem.

藉此，所述未反應單體除去裝置的溫水噴射裝置為重要的裝置，例如於專利文獻2中提議有所述溫水噴射裝置及方法。Therefore, the warm water spray device of the unreacted monomer removal device is an important device, and the warm water spray device and method are proposed in Patent Document 2, for example.

進而，近年來，提議有如專利文獻3至專利文獻5的殘留單體除去裝置，所述殘留單體除去裝置具有：筒狀的塔本體；多個多孔板，設置於所述塔本體的垂直方向上；多個室，分別以所述多孔板為底面而形成於多孔板上方；漿料導入口，設置於所述多個多孔板中最上部的多孔板的上側；流下部，設置於所述多孔板間以使漿料自上方的室的多孔板朝下方的室的多孔板順次流下；水蒸氣導入口，設置於塔本體的底部；凝縮裝置，在塔本體的塔頂室隔著氣體移送管而設置於所述塔本體的外部；漿料排出口，設置於所述多個多孔板中最下部的多孔板；以及溫水噴射裝置，於多孔板的正下方，設置為至少朝向所述多孔板的下表面。Furthermore, in recent years, a residual monomer removal device such as Patent Document 3 to Patent Document 5 has been proposed. The residual monomer removal device has: a cylindrical tower body; and a plurality of perforated plates provided in the vertical direction of the tower body Upper; multiple chambers, each formed on the porous plate with the porous plate as a bottom surface; slurry inlet, provided on the upper side of the uppermost porous plate of the multiple porous plates; the lower flow portion, provided on the porous Between the plates so that the slurry flows down from the porous plate of the upper chamber to the porous plate of the lower chamber in sequence; the water vapor inlet is provided at the bottom of the tower body; the condensation device is in the tower top chamber of the tower body via a gas transfer tube It is provided outside the tower body; the slurry discharge port is provided at the lowest perforated plate among the plurality of perforated plates; and the warm water spraying device is provided directly below the perforated plate, at least toward the porous The lower surface of the board.

其中，在溫水噴射清洗時為了確保適當的溫水噴射量，而需要維持各室的溫水噴射壓力，所述壓力以與設置在各室入口的溫水噴射噴嘴連接的壓力計的指示值成為規定的壓力的方式利用手動閥對開度進行調整。然而，有因溫水泵的出口壓力的變動而無法確保規定的壓力的情形。Among them, in order to ensure an appropriate amount of warm water spray during warm water spray cleaning, it is necessary to maintain the warm water spray pressure of each chamber, the pressure being indicated by the pressure gauge connected to the warm water spray nozzle provided at the entrance of each chamber The opening degree is adjusted by a manual valve so that it becomes a predetermined pressure. However, there may be cases where the predetermined pressure cannot be secured due to the change in the outlet pressure of the warm water pump.

又，在進行未反應單體除去裝置的定期的運轉狀態的確認或運轉變得不穩定時等，為了以目視確認各室內部的漿料水準或鼓泡（bubbling）狀態，而在各室的側面設置有視窗（sight glass），而可觀察內部。然而，對於視窗，有附著有飛散的漿料的情形而內部變得不易觀察。因此將用於清洗視窗的清洗噴嘴自溫水噴射環進行連接，但由於是自溫水噴射環的下側進行連接，因此即便溫水噴射清洗結束，由於溫水自視窗清洗噴嘴滴下而溫水抵於視窗直至溫水噴射環內的溫水排出為止，因此亦無法觀察內部直至溫水噴射環內的溫水排出為止。In addition, in order to confirm the periodic operation state of the unreacted monomer removal device or when the operation becomes unstable, etc., in order to visually confirm the slurry level or bubbling state in each chamber, the A sight glass is provided on the side to observe the inside. However, in the window, the scattered slurry may adhere, and the inside becomes difficult to observe. Therefore, the cleaning nozzle for cleaning the window is connected from the warm water spray ring, but because it is connected from the lower side of the warm water spray ring, even if the warm water spray cleaning is completed, the warm water drops from the window cleaning nozzle and warm water It is against the window until the warm water in the warm water spray ring is discharged, so it is impossible to observe the inside until the warm water in the warm water spray ring is discharged.

進而，在室內溫度與溫水溫度的溫差大時，由於在清洗時室內的溫度發生變動而壓力亦發生變動，因此有引起所述室的上多孔板或下多孔板漏液的情況。 [現有技術文獻] [專利文獻]Furthermore, when the temperature difference between the room temperature and the temperature of the hot water is large, the temperature of the room changes and the pressure also changes during the cleaning, so that the upper or lower porous plate of the chamber may leak liquid. [Prior Art Literature] [Patent Literature]

[專利文獻1]日本專利特開昭54-8693 [專利文獻2]日本專利特開昭56-22305 [專利文獻3] 日本專利特開平6-107723 [專利文獻4]日本專利特開平10-338708 [專利文獻5]日本專利特開平9-48815[Patent Document 1] Japanese Patent Laid-Open No. 54-8693 [Patent Document 2] Japanese Patent Laid-Open No. 56-22305 [Patent Document 3] Japanese Patent Laid-Open No. 6-107723 [Patent Document 4] Japanese Patent Laid-Open No. 10-338708 [Patent Document 5] Japanese Patent Laid-Open No. 9-48815

[發明所欲解決之課題][Problems to be solved by the invention]

需求一種可一面防止於製程外排出未反應單體，且一面自含氯化乙烯系樹脂漿料將殘留單體高效地除去的殘留單體除去裝置。 [解決課題之手段]There is a need for a residual monomer removal device that can prevent unreacted monomers from being discharged outside the manufacturing process and efficiently remove residual monomers from a vinyl chloride-based resin slurry. [Means to solve the problem]

本發明的殘留單體除去裝置的構成如下文所述。其具有：筒狀的塔本體4；多個多孔板34，設置於所述塔本體內的垂直方向上；多個室16～室21，分別以所述多孔板為底面而形成於多孔板上方；漿料導入管22、漿料導入管23；流下管36，使漿料自上方的室的多孔板朝下方順次流下；水蒸氣導入管10，設置於塔本體的底部；凝縮裝置6，於塔本體的上部隔著氣體排出口11而設置；漿料排出口24，設置於最下部的多孔板；以及溫水噴射環38，位於多孔板的正下方；且在包含溫水噴射環的溫水噴射裝置中設置有：壓力計40，用於有效地進行噴射壓力監視；用於調整所述壓力的裝置（壓力控制閥32、或附帶逆變器（inverter）控制功能的溫水泵8）；進而設置有視窗清洗噴嘴37，自溫水噴射裝置的溫水噴射環38上部連接或***環內。The configuration of the residual monomer removal device of the present invention is as follows. It has: a cylindrical tower body 4; a plurality of perforated plates 34, which are provided in the vertical direction of the tower body; a plurality of chambers 16 to 21, each formed on the perforated plate with the perforated plate as the bottom surface; Slurry introduction tube 22, slurry introduction tube 23; flow down tube 36, which makes the slurry flow down sequentially from the porous plate of the upper chamber; water vapor introduction tube 10, provided at the bottom of the tower body; condensing device 6, at the tower The upper part of the body is provided through the gas discharge port 11; the slurry discharge port 24 is provided at the lowermost porous plate; and the warm water spray ring 38 is located directly below the porous plate; and the warm water containing the warm water spray ring The injection device is provided with: a pressure gauge 40 for effectively monitoring the injection pressure; a device for adjusting the pressure (pressure control valve 32, or a warm water pump 8 with an inverter control function); and A window cleaning nozzle 37 is provided, and the upper part of the warm water spray ring 38 of the warm water spray device is connected or inserted into the ring.

為了解決所述課題，本發明包含以下項目。 [1]一種殘留單體除去裝置，其自含有聚合結束後的未反應單體的含聚氯化乙烯的漿料除去未反應單體，且所述殘留單體除去裝置具有：筒狀的塔本體； 多個多孔板，設置於所述塔本體的垂直方向上； 多個室，分別以所述多孔板為底面而形成於多孔板上方； 漿料導入口，設置於所述多個多孔板中最上部的多孔板的上側； 流下部，設置於所述多孔板間以使漿料自上方的室的多孔板朝下方的室的多孔板順次流下； 水蒸氣導入口，設置於塔本體的底部； 凝縮裝置，在塔本體的塔頂室隔著氣體移送管而設置於所述塔本體的外部； 漿料排出口，設置於所述多個多孔板中最下部的多孔板；以及 溫水噴射裝置，於多孔板的正下方，設置為至少朝向所述多孔板的下表面；且所述殘留單體除去裝置中： 在所述溫水噴射裝置中，為了噴射適當的噴射量的溫水而安裝有監視噴射壓力的壓力計、及用於控制所述噴射壓力的裝置。In order to solve the above problems, the present invention includes the following items. [1] A residual monomer removal device that removes unreacted monomers from a polyvinyl chloride-containing slurry containing unreacted monomers after completion of polymerization, and the residual monomer removal device has a cylindrical tower Ontology A plurality of perforated plates are provided in the vertical direction of the tower body; A plurality of chambers are respectively formed above the porous plate with the porous plate as a bottom surface; The slurry introduction port is provided on the upper side of the uppermost porous plate among the multiple porous plates; The lower part of the flow is arranged between the porous plates so that the slurry flows down from the porous plate of the upper chamber to the porous plate of the lower chamber in sequence; The steam inlet is set at the bottom of the tower body; The condensation device is provided outside the tower body through a gas transfer tube in the top chamber of the tower body; A slurry discharge port, which is provided at the lowermost porous plate among the multiple porous plates; and The warm water spraying device is arranged directly below the porous plate at least toward the lower surface of the porous plate; and in the residual monomer removing device: In the warm water injection device, a pressure gauge for monitoring the injection pressure and a device for controlling the injection pressure are installed in order to inject an appropriate injection amount of warm water.

[2]如[1]所述的殘留單體除去裝置，其中用於控制噴射壓力的裝置是壓力控制閥或對溫水供給泵輸出施以逆變器控制化而調節溫水噴射壓力的裝置。[2] The residual monomer removal device according to [1], wherein the device for controlling the injection pressure is a pressure control valve or a device that controls the output of the warm water supply pump by controlling the inverter to adjust the warm water injection pressure .

[3]如[1]或[2]所述的殘留單體除去裝置，其中在所述溫水噴射裝置所具有的溫水噴射環中，具有用於清洗設置於各室1處以上的視窗的清洗噴嘴。[3] The residual monomer removing device according to [1] or [2], wherein the warm water spray ring included in the warm water spray device has a window for cleaning at least one location in each chamber Cleaning nozzle.

[4]如[3]所述的殘留單體除去裝置，其中所述溫水噴射環所具有的用於清洗視窗的清洗噴嘴自所述溫水噴射環的上側連接。[4] The residual monomer removing device according to [3], wherein the cleaning nozzle for cleaning the window provided in the warm water spray ring is connected from the upper side of the warm water spray ring.

[5]如[3]所述的殘留單體除去裝置，其中所述溫水噴射環所具有的用於視窗的清洗的清洗噴嘴以***所述溫水噴射環的內部的方式連接。 [發明的效果][5] The residual monomer removing device according to [3], wherein the cleaning nozzle for cleaning the window included in the warm water spray ring is connected so as to be inserted inside the warm water spray ring. [Effect of invention]

根據[1]或[2]記載的發明，是一種自含有聚合結束後的未反應單體的含聚氯化乙烯的漿料除去未反應單體的除去裝置，為了將溫水噴射裝置中的噴射壓力設為規定的壓力，而可藉由設置壓力控制閥或將溫水泵的輸出施以逆變器控制化來調整溫水噴射壓力。又，藉由使用逆變器，而亦實現節能。According to the invention described in [1] or [2], it is a removal device for removing unreacted monomers from a polyvinyl chloride-containing slurry containing unreacted monomers after completion of polymerization. The injection pressure is set to a predetermined pressure, and the hot water injection pressure can be adjusted by installing a pressure control valve or controlling the output of the warm water pump with an inverter. In addition, by using an inverter, energy saving is also achieved.

根據[3]記載的發明，藉由在所述溫水噴射裝置所具有的溫水噴射環內，設置用於清洗各室的視窗的清洗噴嘴，而可觀察各室的內部狀況。According to the invention described in [3], by arranging a cleaning nozzle for cleaning the window of each chamber in the warm water injection ring included in the warm water injection device, the internal state of each chamber can be observed.

根據[4]或[5]記載的發明，由於將所述溫水噴射環所具有的用於清洗視窗的清洗噴嘴設為自下側***的噴嘴或自溫水噴射環的上側連接，因此無需等待積存於溫水噴射環內的溫水自清洗噴嘴排出，而可觀察各室的內部狀況。又，藉由將溫水預先儲存於溫水噴射環中而室內的溫度與所述溫水噴射環內的溫水溫度的差變小，因此在溫水噴射清洗時室內的壓力變動被緩和，而防止自多孔板漏液。According to the invention described in [4] or [5], since the cleaning nozzle for cleaning the window included in the warm water spray ring is a nozzle inserted from the lower side or connected from the upper side of the warm water spray ring, there is no need Wait for the warm water stored in the warm water spray ring to be discharged from the cleaning nozzle, and observe the internal conditions of each chamber. In addition, by storing the warm water in the warm water spray ring in advance and the difference between the indoor temperature and the warm water temperature in the warm water spray ring becomes small, the pressure fluctuation in the room during the warm water spray cleaning is alleviated, And prevent leakage from the multi-well plate.

在本發明的殘留單體除去裝置中，基於圖1～圖6對自PVC漿料除去殘留單體的方法進行說明，但本發明並不限於此。In the residual monomer removal device of the present invention, the method of removing residual monomers from the PVC slurry will be described based on FIGS. 1 to 6, but the present invention is not limited to this.

1.殘留單體除去裝置的構成 所述裝置具有：筒狀的塔本體4；多個多孔板34，設置於所述塔本體4的垂直方向上，各自具有多個細孔；多個室16～室21，分別以所述多孔板為底面而形成於多孔板上方；作為漿料導入部的漿料導入口22、漿料導入口23，設置於所述多個多孔板中塔頂室21下的多孔板或室19下的多孔板的上側；流下管36，設置於所述多孔板間以使漿料自上方的室的多孔板朝下方的室的多孔板順次流下；水蒸氣導入管10，設置於塔本體的底部；凝縮器6，於塔本體的頂部隔著氣體移送口11而設置；未反應單體氣體移送管12，設置於所述凝縮器出口；PVC漿料排出口24，設置於所述多個多孔板中最下部的多孔板；以及作為溫水噴射機構的溫水噴射環38，於各多孔板的正下方，朝向所述多孔板的正下方而設置。1. Configuration of residual monomer removal device The device has: a cylindrical tower body 4; a plurality of perforated plates 34, provided in the vertical direction of the tower body 4, each having a plurality of fine holes; a plurality of chambers 16 to 21, respectively It is formed above the porous plate for the bottom surface; the slurry introduction port 22 and the slurry introduction port 23 as the slurry introduction part are provided in the porous plate under the tower top chamber 21 or the porous under the chamber 19 among the multiple porous plates The upper side of the plate; the flow-down tube 36 is provided between the porous plates so that the slurry flows down from the porous plate of the upper chamber to the porous plate of the lower chamber in sequence; the water vapor introduction pipe 10 is provided at the bottom of the tower body; condensation 6 is provided at the top of the tower body via a gas transfer port 11; an unreacted monomer gas transfer tube 12 is provided at the outlet of the condenser; a PVC slurry discharge port 24 is provided in the multiple porous plates The lowermost porous plate; and the warm water spray ring 38 as a warm water spray mechanism are provided directly under each porous plate and directly below the porous plate.

1-1.塔本體 塔本體4的內徑為200 mm～10000 mm，塔高度為內徑的2倍～20倍，更佳為5倍～15倍。又，塔內各室的內徑可根據需要而不同。在未反應單體除去處理塔4中，將由塔底與多孔板、多孔板與位於其正上部的多孔板、或多孔板與塔頂所區劃的空間稱為室。用於處理未反應單體而所需的室數藉由自PVC漿料除去未反應單體時所需的滯留時間而決定。1-1. Tower body The inner diameter of the tower body 4 is 200 mm to 10000 mm, and the height of the tower is 2 to 20 times the inner diameter, more preferably 5 to 15 times. In addition, the inner diameter of each chamber in the tower may be different according to needs. In the unreacted monomer removal treatment tower 4, the space partitioned by the bottom of the tower and the porous plate, the porous plate and the porous plate located directly above it, or the porous plate and the top of the tower is called a chamber. The number of chambers required for processing unreacted monomers is determined by the residence time required to remove unreacted monomers from the PVC slurry.

1-2.多孔板 具有多個細孔的多孔板34在各自的表面垂直地設置有數個擋板35，而在與上部的多孔板的下表面之間形成室（空間）。多孔板的細孔是以在PVC漿料在多孔板上流動時藉由自細孔噴入而來的水蒸氣進行脫單體處理的方式而開孔。細孔的大小是以PVC漿料不會穿過細孔而流下，而且不會堵塞細孔，並且自下方噴入而來的水蒸氣連續不斷地均一地穿過的方式考量水蒸氣壓及水蒸氣導入量而設定。1-2. Multi-well plate The porous plate 34 having a plurality of fine holes is provided with a plurality of baffles 35 vertically on the respective surfaces, and a chamber (space) is formed between the lower surface of the upper porous plate. The pores of the perforated plate are formed by demonomerizing the water vapor sprayed from the pores when the PVC slurry flows on the perforated plate. The size of the pores is such that the PVC slurry does not flow through the pores and does not block the pores, and the water vapor sprayed from below continuously and uniformly passes through the water vapor pressure and water vapor. Set the amount of import.

於多孔板開孔的細孔的直徑為5 mm以下，較佳為0.5 mm～2 mm，更佳為0.7 mm～1.5 mm。又，多孔板的開口率（總細孔面積/多孔板面積）為0.001%～10%，較佳為0.04%～4%，更佳為0.2%～2%。 當開口率在此範圍內時，由於在多孔板製擱板上流動的PVC漿料中所存在的PVC粒子被充分地攪拌，因此可防止因PVC粒子沈降所致的源自PVC粒子的未反應單體的除去效率降低及PVC漿料的流動性的降低。又，當開口率在此範圍內時，由於不會產生PCV漿料自細孔流下的現象（以下，稱為漏液），而可防止漏液，因此不會為了防止漏液而浪費大量的水蒸氣量。 擋板35用於確保PVC漿料可在多孔板上流動的處理通路。於多孔板34的上表面，擋板彼此交錯地設置，藉由利用擋板形成的處理通路，而PVC漿料在多孔擱板上流動固定時間，在此期間，接受由自下方供給的水蒸氣進行的脫單體處理。The diameter of the fine holes opened in the porous plate is 5 mm or less, preferably 0.5 mm to 2 mm, and more preferably 0.7 mm to 1.5 mm. In addition, the aperture ratio of the porous plate (total pore area/perforated plate area) is 0.001% to 10%, preferably 0.04% to 4%, and more preferably 0.2% to 2%. When the opening ratio is within this range, since the PVC particles present in the PVC slurry flowing on the perforated shelf are sufficiently stirred, it is possible to prevent unreacted PVC-derived particles due to the precipitation of PVC particles The monomer removal efficiency is reduced and the fluidity of the PVC slurry is reduced. In addition, when the opening ratio is within this range, the phenomenon of PCV slurry flowing down from the pores (hereinafter, referred to as liquid leakage) does not occur, and liquid leakage can be prevented, so a large amount of waste is not wasted in order to prevent liquid leakage The amount of water vapor. The baffle 35 is used to ensure a processing path where PVC slurry can flow on the porous plate. On the upper surface of the perforated plate 34, baffles are alternately arranged with each other. By using the processing passage formed by the baffle, the PVC slurry flows on the perforated shelf for a fixed time, during which time, water vapor supplied from below is received Demonomerization treatment carried out.

1-3.溫水噴射裝置 又，在本發明的未反應單體除去裝置的塔本體4內設置有溫水噴射裝置。作為溫水噴射裝置的溫水噴射環38是將管（pipe）成形為規定的形狀（圖4），且分別設置於多孔板34的正下方，每隔規定時間自噴射噴嘴噴射溫水，而將多孔板的下表面及塔內壁進行清洗。對於噴射噴嘴的數目或噴嘴孔39的位置並無特別限制，但與噴射噴嘴的鉛垂線的交叉角度a、交叉角度b（圖3）較佳為設定在10度～60度的範圍內。 為了對溫水賦予充分的噴出速度以及清洗力，溫水噴出時的溫水噴射環內的壓力與進行所述溫水噴射的室內的壓力的差壓為0.02 MPaG以上，較佳的是在0.05 MPaG以上為恰當。若差壓在此範圍內，則亦不增大溫水消耗量而可獲得充分的清洗效果的溫水噴射的壓力控制能夠藉由對溫水泵8施以逆變器化而使溫水循環線路壓力進行自動控制，或使壓力控制閥32進行自動控制而實施。1-3. Warm water injection device In addition, a warm water injection device is provided in the column body 4 of the unreacted monomer removal device of the present invention. The warm water spray ring 38 as a warm water spray device is formed by forming a pipe into a predetermined shape (FIG. 4 ), and is provided directly under the porous plate 34, and sprays warm water from the spray nozzle every predetermined time, and Clean the lower surface of the perforated plate and the inner wall of the tower. The number of injection nozzles or the position of the nozzle hole 39 is not particularly limited, but the intersection angle a and the intersection angle b (FIG. 3) with the vertical line of the injection nozzle are preferably set within a range of 10 degrees to 60 degrees. In order to give sufficient discharge speed and cleaning power to the warm water, the pressure difference between the pressure in the warm water spray ring during the warm water spray and the pressure in the room where the warm water is sprayed is 0.02 MPaG or more, preferably 0.05 MPaG or higher is appropriate. If the differential pressure is within this range, the pressure control of the hot water spray that can obtain a sufficient cleaning effect without increasing the consumption of the hot water can make the hot water circulation line pressure by applying the inverter to the hot water pump 8 The automatic control is performed, or the pressure control valve 32 is controlled automatically.

1-4.視窗的清洗管 視窗33的清洗管37適當的是如圖5所示自溫水噴射環38的上部連接、或如圖6所示自溫水噴射環38的下部***而連接。當自溫水噴射環的下側連接時，即便清洗結束但殘留於溫水清洗環內的溫水自視窗清洗噴嘴滴落而抵於視窗，因此無法自視窗觀察內部。又，在室內的溫度與溫水的溫度的溫差大時，由於在清洗時室內的溫度發生變動而壓力亦發生變動，因此有引起所述上多孔板或下多孔板漏液的情況。若藉由將視窗清洗管自溫水噴射環的上部連接、或自溫水噴射環的下部***而連接，而將溫水預先儲存於溫水噴射環內，則由於室內與所述環內的溫水的溫差逐漸變小，因此防止多孔板的漏液。1-4. Window cleaning tube The washing tube 37 of the window 33 is suitably connected from the upper portion of the warm water spray ring 38 as shown in FIG. 5 or inserted from the lower portion of the warm water spray ring 38 as shown in FIG. 6. When the lower side of the self-heating water spray ring is connected, even if the cleaning is completed, the warm water remaining in the warm water cleaning ring drops from the window cleaning nozzle and hits the window, so the inside cannot be observed from the window. In addition, when the temperature difference between the temperature in the room and the temperature of the warm water is large, the temperature in the room changes and the pressure changes during the cleaning, so that the upper or lower porous plate may leak liquid. If the window cleaning tube is connected from the upper part of the warm water spray ring or inserted from the lower part of the warm water spray ring, and the warm water is stored in the warm water spray ring in advance, the indoor and the ring The temperature difference of the warm water gradually becomes smaller, thus preventing the leakage of the porous plate.

1-5.溫水噴射環 作為溫水噴射裝置的溫水噴射環38的管的平面形狀通常為希臘文字的Ω型或Φ型、或渦旋型、星形或羊腸型（來回折疊）的樣態，亦可為交互地將中心設為相同的多重環型（圖4）。溫水噴射環38與多孔板34平行地設置，只要收納於塔內部即可，但若過於接近塔本體內壁，則會有被沖洗的PVC粒子等堵塞間隙的擔憂，因此可設置為其外徑處於自塔內壁朝內側隔開20 mm以上的距離。溫水噴射環38的外徑較佳為150 mm～8000 mm。1-5. Warm water jet ring The plane shape of the tube of the warm water spray ring 38 as the warm water spray device is usually the Greek type of Ω type or Φ type, or scroll type, star shape or sheep intestine type (folding back and forth), or alternatively Set the center to the same multi-ring type (Figure 4). The warm water spray ring 38 is provided parallel to the perforated plate 34, as long as it is stored inside the tower, but if it is too close to the inner wall of the tower body, there may be a possibility that the PVC particles, etc., that are washed are blocking the gap, so it can be installed outside The diameter is at a distance of more than 20 mm from the inner wall of the tower toward the inside. The outer diameter of the warm water spray ring 38 is preferably 150 mm to 8000 mm.

2.自PVC漿料除去殘留單體的方法 暫時儲存於PVC漿料槽1的藉由懸濁聚合或乳液聚合而獲得的PVC漿料，藉由PVC漿料供給泵2引導至熱交換器3，在熱交換器3內被加熱至規定溫度後，自PVC漿料導入管22或PVC漿料導入管23導入至未反應單體除去處理塔4內。2. Method for removing residual monomers from PVC slurry The PVC slurry obtained by suspension polymerization or emulsion polymerization temporarily stored in the PVC slurry tank 1 is guided to the heat exchanger 3 by the PVC slurry supply pump 2 and heated to a predetermined temperature in the heat exchanger 3 After that, it is introduced into the unreacted monomer removal treatment tower 4 from the PVC slurry introduction pipe 22 or the PVC slurry introduction pipe 23.

朝塔內導入的PVC漿料的流量較佳的是調整為每1m2 多孔板34的面積為0.1 m3 /h～300 m3 /h（更佳為1 m3 /h～100 m3 /h）。朝塔內導入的PVC漿料理想的是藉由熱交換器3預熱為50 ℃～100 ℃。藉由所述預熱而提高未反應單體除去效率。 自PVC漿料除去單體的難易度取決於PVC漿料中的PVC粒子的構造。於PVC粒子內的細孔容積率大時，因PVC粒子與水蒸氣的接觸良好而易於進行脫單體，於細孔容積率小時，難以進行脫單體。PVC漿料在塔內的滯留時間藉由如上文所述的PVC漿料的脫單體的難易度、導入至塔內的PVC漿料中所含的未反應單體濃度、及在PVC漿料排出口24的處理後的未反應單體濃度的設定值而決定。The flow rate of the PVC slurry introduced into the tower is preferably adjusted to 0.1 m 3 /h to 300 m 3 /h per 1 m 2 perforated plate 34 (more preferably 1 m 3 /h to 100 m 3 / h). The PVC slurry introduced into the tower is preferably preheated by the heat exchanger 3 to 50°C to 100°C. The preheating improves the removal efficiency of unreacted monomers. The ease of removing monomer from the PVC slurry depends on the structure of the PVC particles in the PVC slurry. When the pore volume ratio in the PVC particles is large, demonomerization is easy due to good contact between the PVC particles and water vapor, and when the pore volume ratio is small, it is difficult to perform monomer removal. The residence time of PVC slurry in the tower is determined by the ease of de-monomerization of the PVC slurry as described above, the concentration of unreacted monomers contained in the PVC slurry introduced into the tower, and the PVC slurry The set value of the unreacted monomer concentration after the treatment of the discharge port 24 is determined.

當塔內的PVC漿料的滯留時間長時，可自存在於PVC漿料中的PVC粒子高度地除去未反應單體，但若過長則會引起PVC的粒子因熱劣化所致的著色。因此，PVC漿料欠佳為與必要以上的水蒸氣進行接觸。因此，需要配合PVC漿料的脫單體性的難易度而調整滯留時間。When the residence time of the PVC slurry in the tower is long, unreacted monomers can be highly removed from the PVC particles present in the PVC slurry, but if it is too long, the PVC particles will become colored due to thermal degradation. Therefore, the PVC slurry is not good enough to contact with water vapor more than necessary. Therefore, it is necessary to adjust the residence time in accordance with the difficulty of demonomerization of PVC slurry.

自作為漿料導入部的漿料導入管22或漿料導入管23導入至塔本體內的PVC漿料，經由利用多孔板34上的擋板35區劃的處理通路，穿過流下管36而被導入至其下部的室的多孔板34上。被導入至多孔板34上的漿料繼續經由多孔板34上的處理通路，進而穿過流下管36而朝其下部的多孔板34上流入。如此般在經由最下部的多孔板34為止的處理通路後，自設置於最下部的多孔板34的PVC漿料排出口24排出至塔外。The PVC slurry introduced into the tower body from the slurry introduction pipe 22 or the slurry introduction pipe 23 as a slurry introduction part passes through the downflow tube 36 through the treatment passage partitioned by the baffle plate 35 on the porous plate 34 It is introduced into the porous plate 34 of the lower chamber. The slurry introduced onto the perforated plate 34 continues to pass through the treatment passage on the perforated plate 34 and then passes through the downflow tube 36 to flow into the lower perforated plate 34. In this way, after passing through the treatment passage to the lowermost porous plate 34, the PVC slurry discharge port 24 provided at the lowermost porous plate 34 is discharged to the outside of the tower.

本發明的多孔板34在擋板35的數目或處理通路的寬度上並無特別限制，但因流動的PVC的液面高度增加而超過擋板，而會混入滯留時間不同的PVC漿料，因此為了防止使產品的品質降低，而需要將擋板的數目與處理通路的寬度適當地進行設定。 在本發明的裝置中，將水蒸氣導入管10連接於塔底室15，自水蒸氣導入口10噴射的水蒸氣穿過多孔板的細孔而被吹入在多孔擱板上流動的PVC漿料中。此時的水蒸氣導入量為每1 m3 PVC漿料1 Kg/h～100 Kg/h，較佳為5 Kg/h～50 Kg/h。若水蒸氣導入量在此範圍內，則在PVC漿料中的PVC粒子不會沈降，而可高效率地除去PCV漿料中的未反應單體。又，若水蒸氣導入量在此範圍內，則可抑制PVC漿料產生飛沫，從而不會產生溢流（Flooding）。又，若水蒸氣導入量在此範圍內，則良好地平衡水蒸氣導入量與PVC漿料中的未反應單體的除去效果。The perforated plate 34 of the present invention is not particularly limited in terms of the number of baffles 35 or the width of the processing passages, but due to the increase in the height of the liquid level of the flowing PVC, which exceeds the baffles, PVC slurry with different retention times is mixed in, so In order to prevent the quality of the product from being degraded, it is necessary to appropriately set the number of baffles and the width of the processing passage. In the apparatus of the present invention, the water vapor introduction pipe 10 is connected to the tower bottom chamber 15, and the water vapor ejected from the water vapor introduction port 10 passes through the pores of the porous plate and is blown into the PVC slurry flowing on the porous shelf Expected. The amount of water vapor introduced at this time is 1 Kg/h to 100 Kg/h per 1 m 3 of PVC slurry, preferably 5 Kg/h to 50 Kg/h. If the amount of water vapor introduced is within this range, the PVC particles in the PVC slurry will not settle, and unreacted monomers in the PCV slurry can be efficiently removed. In addition, if the amount of water vapor introduced is within this range, it is possible to suppress the generation of droplets in the PVC slurry, so that flooding does not occur. In addition, if the amount of introduced steam is within this range, the amount of introduced steam and the effect of removing unreacted monomers in the PVC slurry are well balanced.

又，調整PVC漿料的溫度可獲得高品質的PVC。通常，理想的是以在多孔板上流動的漿料的溫度為50 ℃～150 ℃，較佳為70 ℃～120 ℃，更佳為80 ℃～110 ℃的方式調整水蒸氣溫度與水蒸氣導入量及塔內壓力。若PVC漿料的溫度在此範圍內，則可一面維持未反應單體的除去效率，一面防止PVC粒子的因熱劣化所致的著色等，從而維持高品質。In addition, high-quality PVC can be obtained by adjusting the temperature of the PVC slurry. Generally, it is desirable to adjust the water vapor temperature and water vapor introduction in such a manner that the temperature of the slurry flowing on the porous plate is 50°C to 150°C, preferably 70°C to 120°C, and more preferably 80°C to 110°C Volume and pressure in the tower. If the temperature of the PVC slurry is within this range, the removal efficiency of unreacted monomers can be maintained, while the coloring of PVC particles due to thermal degradation can be prevented, and high quality can be maintained.

在未反應單體除去裝置內被除去的單體氣體與水蒸氣的混合氣體經由與塔頂室21連結的氣體移送管流入凝縮器6，在此處大部分的水蒸氣被凝縮，凝縮水落於未反應單體除去處理塔內而被返回。此時，自塔頂室上升而來的單體氣體和水蒸氣的混合氣體與流下的凝縮水對流接觸而凝縮水被加溫。進而，將導入至凝縮器6的冷卻水13自凝縮器6經由冷卻水出口溫水供給管14而朝溫水槽7引導，藉由用作溫水清洗用的溫水而可防止能源的浪費。藉由未反應單體除去處理塔4經除去未反應單體的PVC漿料自PVC漿料排出口24被排出，且被送入泵9。此後，PVC漿料通過熱交換器3並儲存於PVC漿料槽5中。 [實施例]The mixed gas of the monomer gas and water vapor removed in the unreacted monomer removal device flows into the condenser 6 through the gas transfer pipe connected to the top chamber 21, where most of the water vapor is condensed and the condensed water falls on Unreacted monomer is removed from the treatment tower and returned. At this time, the mixed gas of the monomer gas and the water vapor rising from the tower top chamber comes into convection contact with the condensed water flowing down, and the condensed water is heated. Furthermore, the cooling water 13 introduced into the condenser 6 is guided from the condenser 6 to the warm water tank 7 via the cooling water outlet warm water supply pipe 14, and waste of energy can be prevented by being used as warm water for warm water washing. The PVC slurry through which the unreacted monomers are removed by the unreacted monomer removal treatment tower 4 is discharged from the PVC slurry discharge port 24 and sent to the pump 9. Thereafter, the PVC slurry passes through the heat exchanger 3 and is stored in the PVC slurry tank 5. [Example]

以下，利用實施例對本發明具體地進行說明，但本發明並不被所述實施例限定。Hereinafter, the present invention will be specifically described using examples, but the present invention is not limited to the examples.

使用未反應單體除去處理塔中的溫水噴射裝置的溫水噴射製程是在PVC漿料供給中與供給結束後的清洗水供給中進行實施。 又，溫水噴射清洗自下室16朝上室依序進行溫水噴射清洗。若塔頂室的清洗結束，則又開始進行自室16的清洗。對於室15，若在PVC漿料供給中開啟塔底室的溫水噴射清洗閥31而進行溫水噴射清洗，則室15內的溫度降低且壓力亦降低而會引起自上多孔板漏液，因此在PVC漿料供給中不進行溫水噴射清洗。The warm water spraying process using the warm water spraying device in the unreacted monomer removal treatment tower is carried out during the supply of PVC slurry and the supply of washing water after the supply is completed. In addition, the warm water jet cleaning sequentially performs the warm water jet cleaning from the lower chamber 16 toward the upper chamber. When the cleaning of the tower top chamber is completed, the cleaning of the self-chamber 16 is started again. For the chamber 15, if the warm water jet cleaning valve 31 of the tower bottom chamber is opened and the warm water jet cleaning is performed during the supply of PVC slurry, the temperature in the chamber 15 decreases and the pressure also decreases, causing leakage from the upper porous plate. Therefore, in the supply of PVC slurry, warm water spray cleaning is not performed.

[實施例1] （藉由溫水泵輸出的逆變器控制而進行的溫水噴出壓力控制） 1.啟動溫水泵8，將逆變器輸出設為成為可均一地保持溫水槽7內的溫度分佈的循環量的最低值100 m3 /h。 2.在溫水噴射1分鐘前，將溫水循環線路壓力的設定設為用於使溫水噴射壓力與室內壓力的差壓成為適當的值0.05 MPaG至0.08 MPaG的溫水循環線路壓力，而對溫水泵的逆變器輸出進行自動控制。 3.將溫水泵8的逆變器輸出控制切換為手動模式，且將輸出值固定為所述時點的輸出值。然後，將室16的溫水噴射清洗閥30開放8秒鐘。 4.在關閉溫水噴射清洗閥30後，溫水泵8的逆變器輸出返回至成為可均一地保持溫水槽7內的溫度分佈的循環量的最低值100 m3 /h，且保持所述狀態2分鐘～10分鐘。 5.藉由進行與所述2～4相同的操作而進行上一層的溫水噴射清洗閥29的開閉動作，從而對室17及室18下的多孔板下側進行清洗。 6.藉由重覆與所述2～5相同的操作，而自下室朝上室依序進行溫水噴射清洗。[Example 1] (Hot water discharge pressure control by the inverter control of the hot water pump output) 1. Start the hot water pump 8 and set the inverter output to be able to uniformly maintain the temperature in the hot water tank 7 The lowest value of the distributed circulation volume is 100 m 3 /h. 2. Before the hot water injection for 1 minute, set the pressure of the hot water circulation line to the temperature of the hot water circulation line for the pressure difference between the warm water injection pressure and the indoor pressure to an appropriate value of 0.05 MPaG to 0.08 MPaG. The inverter output of the water pump is automatically controlled. 3. Switch the inverter output control of the warm water pump 8 to the manual mode, and fix the output value to the output value at the time point. Then, the warm water jet cleaning valve 30 of the chamber 16 is opened for 8 seconds. 4. After closing the warm water jet cleaning valve 30, the inverter output of the warm water pump 8 returns to a minimum value of 100 m 3 /h which becomes a circulation amount that can uniformly maintain the temperature distribution in the warm water tank 7 and maintain the State 2 minutes to 10 minutes. 5. By performing the same operations as the above 2 to 4, the warm water jet cleaning valve 29 of the upper layer is opened and closed to clean the lower side of the porous plate under the chamber 17 and the chamber 18. 6. By repeating the same operations as the above 2 to 5, the warm water spray cleaning is performed sequentially from the lower chamber to the upper chamber.

[實施例2] （藉由循環壓力控制閥的控制而進行的溫水噴出壓力控制） 1.啟動溫水泵8，將循環壓力控制閥32開度輸出設為全開。 2.在溫水噴射1分鐘前，將溫水循環線路壓力的設定設為用於使溫水噴射壓力與室內壓力的差壓成為適當的壓力的溫水循環線路壓力，而對循環壓力控制閥32開度輸出進行自動控制。 3.將循環壓力控制閥32切換為手動模式，且固定開度輸出值。然後，將室16的溫水噴射清洗閥30開放8秒鐘。 4.在關閉溫水噴射清洗閥30後，將循環壓力控制閥32開度輸出設為全開。且保持所述狀態2分鐘～10分鐘。 5.藉由進行與所述2～4相同的操作而進行上一層的溫水噴射清洗閥29的開閉動作，從而對室17及室18下的多孔板下側進行清洗。 6.藉由重覆與所述2～5相同的操作，而自下室朝上室依序進行溫水噴射清洗。[Example 2] (Warm water discharge pressure control by control of circulation pressure control valve) 1. Start the warm water pump 8 and set the opening output of the circulation pressure control valve 32 to fully open. 2. One minute before the warm water injection, set the warm water circulation line pressure to the warm water circulation line pressure for making the differential pressure between the warm water injection pressure and the indoor pressure appropriate, and open the circulation pressure control valve 32 Degree output is automatically controlled. 3. Switch the circulation pressure control valve 32 to the manual mode and fix the output value of the opening degree. Then, the warm water jet cleaning valve 30 of the chamber 16 is opened for 8 seconds. 4. After closing the warm water jet cleaning valve 30, the opening output of the circulation pressure control valve 32 is set to fully open. And keep the state for 2 minutes to 10 minutes. 5. By performing the same operation as the above 2 to 4, the warm water jet cleaning valve 29 of the upper layer is opened and closed to clean the lower side of the porous plate under the chamber 17 and the chamber 18. 6. By repeating the same operations as the above 2 to 5, the warm water spray cleaning is performed sequentially from the lower chamber to the upper chamber.

[實施例3] （利用自溫水噴射環上部連接的視窗清洗管的清洗） 各室的視窗33的清洗是在進行各室的溫水噴射清洗時同時進行。因視窗清洗管是自溫水噴射環的上部連接，因此若溫水噴射清洗結束，則溫水始終不會自視窗清洗噴嘴滴落。又，由於將溫水預先儲存於溫水噴射環內，因此清洗時的室內與所述環內的溫水的溫差為1℃以下而變小，從而不會產生多孔板的漏液。[Example 3] (Cleaning using the window cleaning tube connected to the upper part of the self-heated water jet ring) The window 33 of each chamber is cleaned at the same time when the warm water jet cleaning of each chamber is performed. Because the window cleaning tube is connected to the upper part of the self-warm water spray ring, if the warm water spray cleaning is completed, the warm water will never drip from the window cleaning nozzle. In addition, since warm water is stored in the warm water spray ring in advance, the temperature difference between the room during washing and the warm water in the ring is 1° C. or less, and the leakage of the porous plate does not occur.

[實施例4] （利用自溫水噴射環下部***而連接的視窗清洗管的清洗） 與實施例3同樣地，若溫水噴射清洗結束，則溫水始終不會自視窗清洗噴嘴滴落。又，不會產生多孔板的漏液。[Example 4] (Washing using the window cleaning tube inserted from the lower part of the warm water jet ring and connected) In the same manner as in Example 3, when the warm water spray cleaning is completed, the warm water will never drip from the window cleaning nozzle. In addition, there is no leakage of liquid from the porous plate.

[比較例1] 在先前的方法中，在溫水噴射清洗時為了確保合適的溫水噴射壓力，而在設置於各室入口的溫水噴射環入口處設置壓力計與手動閥，以各室的壓力的指示值成為規定的壓力0.05 MPaG至0.08 MPaG的方式利用手動閥對開度進行調整。然而，有因溫水泵的出口壓力的變動，而無法確保規定的壓力的情形。進而，在溫水循環線路中為了確保溫水循環壓力而需要在循環返回線路上設置切斷用自動閥，在各室清洗時開放各室的溫水噴射清洗自動閥，且關閉溫水循環切斷閥，但因開閉閥的時機，而引起配管的錘擊，由此引起配管及閥的振動、以及自配管或閥的凸緣洩漏溫水。[Comparative Example 1] In the previous method, in order to ensure an appropriate warm water jet pressure during the warm water jet cleaning, a pressure gauge and a manual valve were installed at the inlet of the warm water jet ring provided at the entrance of each chamber, with the indication value of the pressure of each chamber The opening degree is adjusted by a manual valve so that the predetermined pressure is 0.05 MPaG to 0.08 MPaG. However, there may be cases where the predetermined pressure cannot be secured due to the change in the outlet pressure of the warm water pump. Furthermore, in order to ensure the circulation pressure of the warm water in the warm water circulation line, it is necessary to provide an automatic valve for shutoff on the circulation return line, to open the automatic valve for warm water spray cleaning of each chamber during cleaning of each chamber, and to close the shutoff valve for the warm water circulation However, due to the timing of opening and closing the valve, hammering of the piping is caused, thereby causing vibration of the piping and valve, and warm water leaking from the piping or valve flange.

[比較例2] 關於先前的視窗清洗，由於視窗清洗管連接於溫水噴射環的下側，因此即便溫水噴射清洗結束，但溫水自視窗清洗噴嘴滴落而溫水抵於視窗直至溫水噴射環內的溫水被完全排出為止，從而無法觀察內部。又，由於因室不同而室內與所述環內的溫水的溫差為5℃以上而較大，因此在溫水噴射清洗時產生多孔板的漏液。 [產業上之可利用性][Comparative Example 2] Regarding the previous window cleaning, since the window cleaning tube is connected to the lower side of the warm water spray ring, even though the warm water spray cleaning is completed, the warm water drops from the window cleaning nozzle and the warm water hits the window until the inside of the warm water spray ring Until the warm water is completely discharged, the inside cannot be observed. In addition, since the temperature difference between the room and the warm water in the ring is large due to the difference between the rooms, the leakage of the porous plate occurs during the hot water spray cleaning. [Industry availability]

本發明的殘留單體除去裝置可用於氯化乙烯系樹脂的製造裝置。The apparatus for removing residual monomers of the present invention can be used in an apparatus for producing chlorinated vinyl resins.

1:PVC漿料槽 2:PVC漿料供給泵 3:熱交換器 4:塔本體、未反應單體除去處理塔 5:PVC漿料槽 6:凝縮裝置、凝縮器 7:溫水槽 8:溫水泵 9:泵 10:水蒸氣導入管、水蒸氣導入口 11:氣體排出口、氣體移送口 12:未反應單體氣體移送管 13:冷卻水 14:冷卻水出口溫水供給管 15:塔底室、室 16～20:室 21:塔頂室、室 22、23:PVC漿料導入管、漿料導入管、漿料導入口 24:漿料排出口、PVC漿料排出口 25～30:溫水噴射清洗閥 31:塔底室的溫水噴射清洗閥 32:壓力控制閥、循環壓力控制閥 33:視窗（各室中編號相同） 34:多孔板（各室中編號相同） 35:擋板（各室中編號相同） 36:流下管（各室中編號相同） 37:視窗清洗噴嘴、清洗管（各室中編號相同） 38:溫水噴射環（各室中編號相同） 39:噴嘴孔 40:壓力計 a、b:交叉角度1: PVC slurry tank 2: PVC slurry supply pump 3: heat exchanger 4: Tower body, unreacted monomer removal treatment tower 5: PVC slurry tank 6: Condensation device, condenser 7: Warm water tank 8: warm water pump 9: Pump 10: Water vapor inlet pipe, water vapor inlet 11: Gas discharge port, gas transfer port 12: Unreacted monomer gas transfer tube 13: Cooling water 14: Warm water supply pipe for cooling water outlet 15: Tower bottom room, room 16～20: room 21: Tower top room, room 22, 23: PVC slurry introduction tube, slurry introduction tube, slurry introduction port 24: slurry outlet, PVC slurry outlet 25～30: Warm water jet cleaning valve 31: Warm water jet cleaning valve in the tower bottom chamber 32: Pressure control valve, circulation pressure control valve 33: Windows (same number in each room) 34: Multi-well plate (same number in each room) 35: Baffle (same number in each room) 36: Downflow tube (same number in each room) 37: Window cleaning nozzle and cleaning tube (same number in each room) 38: Warm water jet ring (same number in each room) 39: Nozzle hole 40: pressure gauge a, b: cross angle

圖1是未反應單體除去裝置的概略圖。 圖2是未反應單體除去處理塔室內的詳圖。 圖3是溫水噴射環放大縱剖面圖。 圖4是自上表面觀察的溫水噴射環整體圖。 圖5是自溫水噴射環上部連接的視窗清洗管的縱剖面圖。 圖6是自溫水噴射環的下部***而連接的視窗清洗管的縱剖面圖。FIG. 1 is a schematic diagram of an unreacted monomer removal device. Fig. 2 is a detailed view of the unreacted monomer removal processing chamber. Fig. 3 is an enlarged longitudinal cross-sectional view of a warm water spray ring. Fig. 4 is an overall view of the warm water spray ring viewed from the upper surface. Fig. 5 is a longitudinal sectional view of a window cleaning tube connected from the upper part of the warm water spray ring. 6 is a longitudinal cross-sectional view of a window cleaning tube inserted and connected from the lower part of the warm water spray ring.

1:PVC漿料槽 1: PVC slurry tank

2:PVC漿料供給泵 2: PVC slurry supply pump

3:熱交換器 3: heat exchanger

4:塔本體、未反應單體除去處理塔 4: Tower body, unreacted monomer removal treatment tower

5:PVC漿料槽 5: PVC slurry tank

6:凝縮裝置、凝縮器 6: Condensation device, condenser

7:溫水槽 7: Warm water tank

8:溫水泵 8: warm water pump

9:泵 9: Pump

10:水蒸氣導入管 10: Water vapor introduction pipe

11:氣體排出口、氣體移送口 11: Gas discharge port, gas transfer port

12:未反應單體氣體移送管 12: Unreacted monomer gas transfer tube

13:冷卻水 13: Cooling water

14:冷卻水出口溫水供給管 14: Warm water supply pipe for cooling water outlet

15:塔底室、室 15: Tower bottom room, room

16~20:室 16~20: room

21:塔頂室、室 21: Tower top room, room

22、23:PVC漿料導入管、漿料導入管、漿料導入口 22, 23: PVC slurry introduction tube, slurry introduction tube, slurry introduction port

24:漿料排出口、PVC漿料排出口 24: slurry outlet, PVC slurry outlet

25~30:溫水噴射清洗閥 25~30: Warm water jet cleaning valve

31:塔底室的溫水噴射清洗閥 31: Warm water jet cleaning valve in the tower bottom chamber

32:壓力控制閥、循環壓力控制閥 32: Pressure control valve, circulation pressure control valve

40:壓力計 40: pressure gauge

Claims (5)

一種殘留單體除去裝置，其自含有聚合結束後的未反應單體的含聚氯化乙烯的漿料除去未反應單體，且所述殘留單體除去裝置具有： 筒狀的塔本體； 多個多孔板，設置於所述塔本體的垂直方向上； 多個室，分別以所述多孔板為底面而形成於所述多孔板上方； 漿料導入口，設置於多個所述多孔板中最上部的所述多孔板的上側； 流下部，設置於所述多孔板間以使所述漿料自上方的所述室的所述多孔板朝下方的所述室的所述多孔板順次流下； 水蒸氣導入口，設置於所述塔本體的底部； 凝縮裝置，在所述塔本體的塔頂室隔著氣體移送管設置於所述塔本體的外部； 漿料排出口，設置於多個所述多孔板中最下部的所述多孔板；以及 溫水噴射裝置，於所述多孔板的正下方，設置為至少朝向所述多孔板的下表面， 所述殘留單體除去裝置的特徵在於： 於所述溫水噴射裝置中，為了噴射適當的噴射量的溫水而安裝有監視噴射壓力的壓力計、及用於控制所述噴射壓力的裝置。A residual monomer removal device that removes unreacted monomers from a polyvinyl chloride-containing slurry containing unreacted monomers after the completion of polymerization, and the residual monomer removal device has: Tubular tower body; A plurality of perforated plates are provided in the vertical direction of the tower body; A plurality of chambers are respectively formed above the porous plate with the porous plate as a bottom surface; The slurry introduction port is provided on the upper side of the uppermost porous plate among the multiple porous plates; The lower part of the flow is arranged between the porous plates so that the slurry flows down from the porous plate of the chamber above to the porous plate of the chamber below; The water vapor inlet is provided at the bottom of the tower body; A condensation device, which is arranged outside the tower body via a gas transfer tube in the tower top chamber of the tower body; A slurry discharge port provided in the lowest part of the plurality of porous plates; and The warm water spraying device is arranged directly below the porous plate at least toward the lower surface of the porous plate, The residual monomer removal device is characterized by: In the warm water injection device, a pressure gauge for monitoring the injection pressure and a device for controlling the injection pressure are installed in order to inject an appropriate injection amount of warm water. 如申請專利範圍第1項所述的殘留單體除去裝置，其中用於控制所述噴射壓力的所述裝置是壓力控制閥或將溫水供給泵輸出施以逆變器控制化而調節溫水噴射壓力的裝置。The residual monomer removal device as described in item 1 of the patent application range, wherein the device for controlling the injection pressure is a pressure control valve or the output of the warm water supply pump is controlled by an inverter to regulate the warm water Spray pressure device. 如申請專利範圍第1項或第2項所述的殘留單體除去裝置，其中於所述溫水噴射裝置所具有的溫水噴射環中，具有用於清洗設置於各所述室1處以上的視窗的清洗噴嘴。The residual monomer removing device according to the first or second patent application scope, wherein the warm water spray ring included in the warm water spray device has one or more cleaning units installed in each of the chambers Nozzle for cleaning windows. 如申請專利範圍第3項所述的殘留單體除去裝置，其中所述溫水噴射環所具有的用於清洗所述視窗的所述清洗噴嘴自所述溫水噴射環的上側連接。The residual monomer removing device according to item 3 of the patent application range, wherein the cleaning nozzle for cleaning the window provided in the warm water spray ring is connected from the upper side of the warm water spray ring. 如申請專利範圍第3項所述的殘留單體除去裝置，其中所述溫水噴射環所具有的用於所述視窗的清洗的所述清洗噴嘴以***所述溫水噴射環的內部的方式連接。The residual monomer removing device according to item 3 of the patent application range, wherein the cleaning nozzle for cleaning the window provided in the warm water spray ring is inserted into the interior of the warm water spray ring connection.
TW108118307A 2018-06-07 2019-05-28 Device for residual-monomer removal TW202012461A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2018-109500 2018-06-07
JP2018109500 2018-06-07

Publications (1)

Publication Number Publication Date
TW202012461A true TW202012461A (en) 2020-04-01

Family

ID=68769549

Family Applications (1)

Application Number Title Priority Date Filing Date
TW108118307A TW202012461A (en) 2018-06-07 2019-05-28 Device for residual-monomer removal

Country Status (6)

Country Link
JP (1) JPWO2019235504A1 (en)
KR (1) KR20210018991A (en)
CN (1) CN111918884B (en)
AU (1) AU2019280943B2 (en)
TW (1) TW202012461A (en)
WO (1) WO2019235504A1 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20220011960A (en) * 2020-07-22 2022-02-03 한화솔루션 주식회사 Residual monomer removal device

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS548693A (en) 1977-06-21 1979-01-23 Chisso Corp Removal of monomer from vinyl chloride resin slurry by steam treatment using improved plate column
JPS5622305A (en) 1979-08-01 1981-03-02 Chisso Corp Monomer removal from vinyl chloride resin slurry by steaming and apparatus therefor
JP3029075B2 (en) 1992-09-25 2000-04-04 チッソ株式会社 Method and apparatus for producing resin powder with low residual vinyl monomer content by steam treatment of vinyl chloride resin slurry
JPH0938602A (en) * 1995-07-31 1997-02-10 Sanyo Electric Co Ltd Washing machine
JP3724012B2 (en) 1995-08-04 2005-12-07 チッソ株式会社 Residual monomer removal apparatus and residual monomer removal method using the same
JPH10338708A (en) * 1997-06-06 1998-12-22 Chisso Corp Apparatus for removing unreacted monomer from polyvinyl chloride-containing slurry and removal
JPH11100410A (en) * 1997-09-29 1999-04-13 Nippon Zeon Co Ltd Operation for recovering unreacted monomer from vinyl chloride polymer latex
KR100338708B1 (en) 1997-12-17 2002-09-05 주식회사 포스코 Method for improving the surface gloss of austenitic stainless bright annealing steel plates
JP2006160845A (en) * 2004-12-06 2006-06-22 Asahi Kasei Chemicals Corp Method for producing water-absorbing resin
JP2008145096A (en) * 2006-11-17 2008-06-26 Chugoku Electric Power Co Inc:The Hot water supply system and hot water supply method
JP6166895B2 (en) * 2012-12-28 2017-07-19 株式会社モリタホールディングス Hot water supply device
JP6783122B2 (en) * 2016-11-24 2020-11-11 大阪瓦斯株式会社 Hot water supply device with mist function

Also Published As

Publication number Publication date
WO2019235504A1 (en) 2019-12-12
AU2019280943A1 (en) 2020-11-12
CN111918884B (en) 2023-05-16
AU2019280943B2 (en) 2024-06-13
JPWO2019235504A1 (en) 2021-06-10
KR20210018991A (en) 2021-02-19
CN111918884A (en) 2020-11-10

Similar Documents

Publication Publication Date Title
JP3709568B2 (en) Residual monomer removal treatment method and residual monomer removal treatment tower used therefor
JP3978797B2 (en) Residual monomer removal method and apparatus
JP3724012B2 (en) Residual monomer removal apparatus and residual monomer removal method using the same
NO771138L (en) PROCEDURES FOR THE REMOVAL OF NON-REAGENTED MONOMES FROM AUTHORIC DISPERSION OF VINYLCHLORIDE POLYMERIZE AND DEVICE FOR CARRYING OUT PROCEDURES
TW202012461A (en) Device for residual-monomer removal
US5250151A (en) Method of evaporating liquids
US4369092A (en) Process for removing monomer from vinyl chloride resin slurry by steam treatment and apparatus employed therefor
KR101319234B1 (en) Process for preparing polybutadiene latex
EA003624B1 (en) An apparatus for evaporative cooling of a liquiform product
JP3162525B2 (en) Continuous treatment method for removing residual monomer from aqueous latex of synthetic polymer and apparatus for performing the same
JP3029075B2 (en) Method and apparatus for producing resin powder with low residual vinyl monomer content by steam treatment of vinyl chloride resin slurry
CN113600583A (en) Full-automatic acid cleaning device and method for glassware
US5151154A (en) Evaporation assembly with vapor circulating means
CN206240094U (en) Integrate the tobacco extract enrichment facility of antiscale, scale removal
CN111504083A (en) Steam ejector suitable for superheated steam
JPH10338708A (en) Apparatus for removing unreacted monomer from polyvinyl chloride-containing slurry and removal
KR850000152B1 (en) Process for extraction of monomer in pvc slurry
SU1693031A1 (en) Juice desulfitation apparatus
JPH11100410A (en) Operation for recovering unreacted monomer from vinyl chloride polymer latex
Love et al. Wetting rates and feed rings in evaporators.
TH2001006491A (en) A device for the removal of residual monomers.
CN109701936A (en) A kind of circulation trough body structure
JP2000327711A (en) Removal of unreacted monomer of polymer solution
JP2002114816A (en) Method and apparatus for removing unreacted vinyl chloride-based monomer