WO2020130264A1 - Manufacturing method and device for aromatic vinyl compound-vinyl cyanide compound polymer - Google Patents

Manufacturing method and device for aromatic vinyl compound-vinyl cyanide compound polymer Download PDF

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Publication number
WO2020130264A1
WO2020130264A1 PCT/KR2019/009587 KR2019009587W WO2020130264A1 WO 2020130264 A1 WO2020130264 A1 WO 2020130264A1 KR 2019009587 W KR2019009587 W KR 2019009587W WO 2020130264 A1 WO2020130264 A1 WO 2020130264A1
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Prior art keywords
condenser
aromatic vinyl
organic solvent
compound
volatile components
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PCT/KR2019/009587
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French (fr)
Korean (ko)
Inventor
황정아
신대영
장성근
주은정
이원균
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(주) 엘지화학
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Priority claimed from KR1020190072784A external-priority patent/KR102435545B1/en
Application filed by (주) 엘지화학 filed Critical (주) 엘지화학
Priority to US16/634,094 priority Critical patent/US11512153B2/en
Priority to JP2020502104A priority patent/JP6998447B2/en
Priority to CN201980003688.XA priority patent/CN111587262B/en
Priority to EP19824186.1A priority patent/EP3689923B1/en
Publication of WO2020130264A1 publication Critical patent/WO2020130264A1/en

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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
    • C08F212/00—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 an aromatic carbocyclic ring
    • C08F212/02—Monomers containing only one unsaturated aliphatic radical
    • C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F212/06—Hydrocarbons
    • C08F212/08—Styrene
    • C08F212/10—Styrene with nitriles
    • 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

Definitions

  • the present invention relates to a method and an apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer, and more specifically, polymerization comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent. Separating volatile components from the product using a volatilization tank; And condensing the separated volatile components using one or two or more condensers connected in series.
  • a method for producing an aromatic vinyl compound-vinyl cyan compound polymer comprising: volatile being separated from the volatilization tank and being transferred to a condenser Spraying an organic solvent over the ingredients; Or spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser when using two or more condensers connected in series; including reducing residual monomers and organic solvents.
  • a method for producing an aromatic vinyl compound-vinyl cyan compound polymer and a manufacturing apparatus comprising: volatile being separated from the volatilization tank and being transferred to a condenser Spraying an organic solvent over the ingredients; Or spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser when using two or more condensers connected in series; including reducing residual monomers and organic solvents.
  • the aromatic vinyl compound-vinyl cyan compound polymer has excellent moldability, stiffness, and electrical properties, and various industries including OA devices such as computers, printers, copiers, home appliances such as televisions, audio, electrical and electronic components, and miscellaneous goods. Widely used in the field. Particularly, the aromatic vinyl compound-vinyl cyan compound polymer that increases heat resistance and withstands high external temperatures is used for special purposes such as for home appliance housings and automobile interior materials.
  • the aromatic vinyl compound-vinyl cyan compound polymer is obtained by reacting an aromatic vinyl compound and a vinyl cyan compound under an organic solvent. At this time, residual monomers and organic solvents remain in addition to the aromatic vinyl compound-vinyl cyan compound polymer in the polymerization product produced after the reaction. Therefore, the process of removing it is essential.
  • the discharged polymerization product is transferred to a volatilization tank to separate volatile components such as residual monomers and organic solvents from the aromatic vinyl compound-vinyl cyan compound polymer, and the separated volatile components are condensed using a condenser, and the aromatic vinyl compound -The vinyl cyan compound polymer becomes a final product after the purification step.
  • the condenser is generally composed of 2 to 3, and the higher the pressure in the condenser, the lower the temperature of the refrigerant increases, but the amount of condensation increases. This will be discharged. In addition, the more the vinyl cyanide monomer having a low boiling point, the lower the condensation efficiency.
  • Volatile components that are not condensed in the condenser are discharged after treatment in a wastewater treatment system or discharged to the atmosphere, and accordingly, a high cost is consumed and the volatile components discharged cause environmental pollution problems.
  • Patent Document 1 Korean Patent Publication No. 10-2007-0073028
  • the present disclosure separates volatile components using a volatilization tank for a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent. To do; And condensing the separated volatile components by using one or two or more condensers connected in series, wherein the method of producing an aromatic vinyl compound-vinyl cyan compound polymer is separated from the volatile tank and being transported to a condenser.
  • An object of the present invention is to provide a method for producing an aromatic vinyl compound-vinyl cyan compound polymer and a manufacturing apparatus.
  • the present invention comprises the steps of separating a volatile component using a volatilization tank for a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent; And condensing the separated volatile components using one or two or more condensers connected in series.
  • a method for producing an aromatic vinyl compound-vinyl cyan compound polymer comprising: volatile being separated from the volatilization tank and being transferred to a condenser Spraying an organic solvent over the ingredients; Or when using two or more condensers connected in series, spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser. It provides a method for producing a vinyl cyan compound polymer.
  • the present disclosure is a volatilization tank for separating a volatile component from a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent; And one or more condensers connected in series to condense the separated volatile components; an apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer, comprising: organic in a transport pipe for transferring the separated volatile components to a condenser.
  • an organic solvent or aromatic vinyl monomer is added to the volatile component being transferred to the first condenser without replacement of the equipment, or to the volatile component not being condensed from the first condenser and being transferred to the second condenser.
  • FIG. 1 is a view schematically showing a step of separating and condensing volatile components from a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, residual aromatic vinyl monomer and an organic solvent according to the present disclosure.
  • FIG. 2 is a view schematically showing a step of separating and condensing a volatile component from a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, residual aromatic vinyl monomer and an organic solvent according to the prior art.
  • the present inventors condenser By introducing an organic solvent or a monomer to the volatile component being transported to the furnace, the condensation efficiency is increased to confirm the effect that the volatile component is discharged without being condensed, and based on this, the study was further conducted to complete the present invention.
  • a volatile component of a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent is volatilized. Separating; And condensing the separated volatile components using one or two or more condensers connected in series.
  • a method for producing an aromatic vinyl compound-vinyl cyan compound polymer comprising: volatile being separated from the volatilization tank and being transferred to a condenser Spraying an organic solvent over the ingredients; Or when using two or more condensers connected in series, spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser.
  • the condensation efficiency is increased, and the volatile components discharged are significantly reduced.
  • the first condenser and the second condenser mean a condenser of a previous stage and a condenser of a later stage between any two condensers of two or more condensers connected in series.
  • the method for producing an aromatic vinyl compound-vinyl cyan compound polymer of the present disclosure uses a volatilization tank for a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent. Separating volatile components; And condensing the separated volatile components using two or more condensers connected in series.
  • a method for producing an aromatic vinyl compound-vinyl cyan compound polymer comprising: volatile being separated from the volatilization tank and being transported to a first condenser.
  • the method for producing the aromatic vinyl compound-vinyl cyan compound polymer includes, for example, spraying an organic solvent to a volatile component separated from the volatile tank and being transferred to a first condenser; And spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not being condensed in the first condenser and is being transferred to the second condenser; in this case, the condensation efficiency is increased and the volatile component discharged is significantly reduced. There is.
  • a step of polymerizing the aromatic vinyl compound and the vinyl cyan compound before the step of separating the volatile components may be included.
  • the aromatic vinyl compound-vinyl cyan compound polymer may be prepared, for example, by reacting an aromatic vinyl compound and a vinyl cyan compound under an organic solvent.
  • the polymerization reaction may include, for example, one or more selected from the group consisting of an initiator, a molecular weight modifier, and an emulsifier.
  • the reaction may be, for example, a bulk polymerization method, a solution polymerization method or an emulsion polymerization method, preferably a bulk polymerization method or a solution polymerization method, and in this case, the tensile strength and impact strength of the aromatic vinyl compound-vinyl cyan compound polymer prepared in this case. It has excellent mechanical properties, heat resistance, and thermal stability.
  • a method for reacting to obtain an aromatic vinyl compound-vinyl cyan compound polymer is not particularly limited, and a commonly used polymerization method can be used.
  • the step of separating volatile components from the volatilization tank may be performed under the conditions of 220 to 260°C and 35 torr or less, preferably 225 to 255°C and 15 to 35 torr, for example, and within this range, volatile components and aromatics There is an effect that the separation of the vinyl compound-vinyl cyan compound polymer is smoothly performed.
  • the volatile tank is not particularly limited when the volatile tank is generally used in the technical field to which the present invention belongs, and a volatile tank that is generally applied may be used.
  • the separated volatile component may include, for example, 5 to 35% by weight of a vinyl cyan compound, 45 to 80% by weight of an aromatic vinyl compound, and 5 to 50% by weight of an organic solvent.
  • the separated volatile component contains 5 to 20% by weight of a vinyl cyan compound, 45 to 59% by weight of an aromatic vinyl compound and 25 to 45% by weight of an organic solvent, or 15 to 35% by weight of a vinyl cyan compound, an aromatic vinyl compound 60 to 80% by weight and 5 to 25% by weight of an organic solvent.
  • the aromatic vinyl compound-vinyl cyan compound polymer that has passed through the volatilization tank may be, for example, transferred to a pelletizer, cut, cooled and dried to obtain pellets.
  • the condenser is preferably two or more condensers connected in series or two condensers can be connected in series, in this case there is an effect that the condensing efficiency is increased.
  • the condenser in the present description is not particularly limited when the condenser is generally used in the technical field to which the present invention belongs, and a condenser that is generally applied may be used.
  • the step of spraying the organic solvent to the volatile components separated from the volatilization tank and being transported to the first condenser is, for example, an organic solvent flow rate of 10 to 200 kg/hr, 10 to 150 kg/hr, or 15 to 100 kg/hr , Preferably it can be sprayed at 15 to 90 kg/hr, more preferably 20 to 50 kg/hr, and in this case, the content ratio of the residual vinyl cyan monomer having a low boiling point in the volatile component is reduced to increase condensation efficiency. It works.
  • the step of spraying the organic solvent to the volatile component being separated from the volatilization tank and being transported to the first condenser for example, the temperature of the organic solvent is -10 °C to 40 °C, preferably 0 to 30 °C, more preferably 15 °C It can be sprayed in the range of 25 to 25 °C, there is an effect that condensation efficiency is increased within this range.
  • the temperature of the organic solvent sprayed to the first condenser is not particularly limited.
  • the step of spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser is, for example, an organic solvent or an aromatic vinyl monomer flow rate of 10 to 200 kg/hr, or 10 to 110 It can be sprayed at kg/hr, preferably 10 to 90 kg/hr, more preferably 10 to 40 kg/hr, and in this case, the content ratio of the residual vinyl cyan monomer having a low boiling point in the volatile component is reduced, thereby condensing efficiency. This increases the effect.
  • the flow rate can be measured by a flow meter or calculated by mass balance.
  • the non-condensed flow rate may be calculated as an input amount-production amount-recovery amount using the mass balance formula.
  • the step of spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and being transported to the second condenser is, for example, an organic solvent or an aromatic vinyl monomer temperature -10 °C to 40 °C, preferably 0 °C to 30 °C, more preferably can be sprayed in the range of 15 °C to 25 °C, there is an effect that increases the condensing efficiency within this range.
  • the temperature of the organic solvent or aromatic vinyl monomer sprayed to the second condenser is not particularly limited.
  • the condensation in the first condenser is, for example, a refrigerant temperature of 20°C to 35°C and an operating pressure of 3 to 100 torr, preferably a refrigerant temperature of 25°C to 33°C and an operating pressure of 15 to 35 torr, more preferably of a refrigerant temperature. 25 °C to 30 °C and can be carried out under the operating pressure of 15 to 30 torr conditions, there is an effect of increasing the condensation efficiency within this range.
  • the operating pressure of the condenser means the internal pressure of the condenser applied when operating the condenser.
  • Condensation in the second condenser is, for example, the refrigerant temperature is -3 °C to 4 °C and the operating pressure 5 to 50 torr condition, preferably the refrigerant temperature is -1 °C to 4 °C and the operating pressure 7 to 25 torr condition, more preferably
  • the refrigerant temperature may be performed under conditions of 0°C to 4°C and an operating pressure of 10 to 20 torr, and there is an effect of increasing condensation efficiency within this range.
  • the condensate condensed from the first condenser and the second condenser can be recovered and purified, for example, and re-entered into the reactor, and in this case, the raw material cost is reduced.
  • Volatile components that are not condensed in the second condenser are transferred to a vacuum unit, for example, dissolved in a circulating fluid of a water-cooled pump and discharged after a wastewater treatment step, and in this process, some may be released into the atmosphere. In this case, in this case, the volatile components released into the atmosphere are significantly reduced, thereby preventing environmental pollution.
  • the organic solvent may be, for example, one or more selected from the group consisting of toluene, ethyl benzene, xylene, methyl ethyl ketone and methyl isobutyl ketone, preferably the organic solvent used in the polymerization reaction and the organic solvent sprayed Is the same, and in this case, by adding a component having a high boiling point in the volatile component, the content ratio of the component having a low boiling point, that is, the residual vinyl cyan monomer is lowered, thereby improving condensation efficiency.
  • the aromatic vinyl compound may be, for example, one or more selected from the group consisting of styrene, ⁇ -methyl styrene, p-methyl styrene, p-bromostyrene, p-chlorostyrene and o-bromostyrene, in this case volatile There is an effect that the condensation efficiency is improved by lowering the content ratio of the residual vinyl cyan monomer in the component having a low boiling point.
  • the apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer of the present invention includes a volatilization tank for separating volatile components from a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, residual aromatic vinyl monomer, residual vinyl cyan monomer and organic solvent; And one or more condensers connected in series to condense the separated volatile components; an apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer, comprising: organic in a transport pipe for transferring the separated volatile components to a condenser.
  • Spraying means for spraying a solvent, or spraying an organic solvent or an aromatic vinyl monomer to a transfer pipe that transports volatile components that are not condensed from the first condenser to the second condenser when including two or more condensers connected in series. It characterized in that it comprises a spray means, in this case, the condensation efficiency is improved, there is an effect that almost no volatile components are discharged after condensation.
  • the spray means is not particularly limited in the case of a means capable of spraying an organic solvent or an aromatic vinyl monomer into the transfer pipe and connected to the transfer pipe, and may be, for example, a spray pipe, a spray container, or the like, and include a spray nozzle. Can.
  • the apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer of the present disclosure separates volatile components from a polymerization product including an aromatic vinyl compound-vinyl cyan compound polymer, residual aromatic vinyl monomer, residual vinyl cyan monomer, and organic solvent. Volatilization; And two or more condensers connected in series to condense the separated volatile components.
  • An aromatic vinyl compound-vinyl cyan compound polymer manufacturing apparatus comprising: an organic solvent in a transport pipe for transferring the separated volatile components to a first condenser.
  • the apparatus for manufacturing the aromatic vinyl compound-vinyl cyan compound polymer includes, for example, a spray pipe for spraying an organic solvent to a transport pipe for transporting the separated volatile component to the first condenser, and the volatile component not condensed in the first condenser It may include a spray pipe for spraying an organic solvent or an aromatic vinyl monomer in the transfer pipe to the second condenser, in which case the condensation efficiency is improved so that there is almost no volatile components discharged after condensation in the second condenser It works.
  • the spray pipe may include, for example, a nozzle.
  • the nozzle of the present invention is a nozzle generally used in the technical field to which the present invention belongs, it is not particularly limited and a nozzle that is generally applied may be used.
  • FIGS. 1 and 2 A method and an apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer according to the present invention will be described with reference to FIGS. 1 and 2 below.
  • FIGS. 1 and 2 These drawings are only schematic diagrams illustrating the present invention and are not limited to the depicted embodiments, and merely depict the means necessary to describe the present invention for ease of understanding, and other obvious means necessary to perform the methods and apparatus are Omitted from the drawings.
  • a volatilization tank (DV), a first condenser (1 st CN), a second condenser (2 nd CN), a vacuum unit, a transport piping used in Examples 1 to 21 according to the present invention
  • a spray pipe a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent is separated from a volatile component in a volatilization tank, and the separated volatile component Spray the organic solvent through the spray pipe to the transfer pipe to the first condenser, or organic solvent or aromatic vinyl monomer to the transfer pipe to transfer the volatile components not condensed from the first condenser to the second condenser through the spray pipe It shows a manufacturing apparatus including spraying.
  • the volatile components that are not condensed in the second condenser are transferred to a vacuum unit, dissolved in the circulating fluid of the water-cooled pump, discharged by treatment with waste water or discharged to the atmosphere.
  • condensate condensed from the first condenser and the second condenser may be re-entered into the reactor.
  • FIG. 2 schematically shows the volatile tank (DV), the first condenser (1 st CN), the second condenser (2 nd CN) and the vacuum unit (Vacuum Unit) used in Comparative Examples 1, 8 and 12
  • a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, and an organic solvent is separated from a volatile component in a volatilization tank and condensed through a first condenser and a second condenser, and in a second condenser
  • the non-condensed volatile components are transferred to a vacuum unit, compressed through a pump, dissolved in a circulating fluid of a water-cooled pump, treated as wastewater, and discharged or discharged to the atmosphere.
  • the condensate condensed in the first condenser and the second condenser may be re-entered into the reactor.
  • Separation condition B temperature 250 °C, pressure was performed under the conditions of 30 torr, at this time, the volatile components separated from the volatilization tank included 68.2% by weight of styrene monomer, 23.7% by weight of acrylonitrile monomer and 9.1% by weight of toluene.
  • Separation conditions C temperature 240 °C, the pressure was carried out under the conditions of 20 torr, at this time, the volatile components separated from the volatilization tank included 62% by weight of styrene monomer, 15% by weight of acrylonitrile monomer and 23% by weight of toluene.
  • Condensation condition A The first condenser was performed under the condition of the refrigerant temperature of 30°C and the pressure of 20 torr, and the second condenser was performed under the refrigerant temperature of 2°C and the pressure of 10 torr.
  • Condensation condition B The first condenser was performed under the condition of the refrigerant temperature of 30°C and the pressure of 30 torr, and the second condenser was performed under the condition of the refrigerant temperature of 2°C and the pressure of 20 torr.
  • Condensation condition C The first condenser was performed under the condition of a refrigerant temperature of 25°C and a pressure of 15 torr, and the second condenser was performed under a refrigerant temperature of -1°C and a pressure of 10 torr.
  • the separated volatile components were condensed to the first condenser under the condensation condition A, and then the uncondensed volatile components were transferred to the second condenser and condensed.
  • toluene was sprayed at a flow rate of 45 kg/hr to the volatile components separated from the volatile tank and being transported to the first condenser, and volatile components not condensed in the first condenser and being transported to the second condenser were not sprayed.
  • the separated volatile components were condensed to the first condenser under the condensation condition A, and then the uncondensed volatile components were transferred to the second condenser and condensed.
  • the volatile components separated from the volatile tank were not sprayed on the volatile components being transferred to the first condenser, and styrene was sprayed on the volatile components not being condensed on the first condenser and being transferred to the second condenser at a flow rate of 30 kg/hr. .
  • the separated volatile components were condensed to the first condenser under the condensation condition A, and then the uncondensed volatile components were transferred to the second condenser and condensed.
  • the volatile component separated from the volatilization tank is not sprayed on the volatile component being transferred to the first condenser, and ⁇ -methyl styrene is flowed to the volatile component that is not condensed on the first condenser and is being transferred to the second condenser at a flow rate of 30 kg/hr. Was sprayed with.
  • the separated volatile components were condensed to the first condenser under the condensation condition A, and then the uncondensed volatile components were transferred to the second condenser and condensed.
  • the volatile components separated from the volatile tank were not sprayed on the volatile components being transferred to the first condenser, and toluene was sprayed on the volatile components not being condensed on the first condenser and being transferred to the second condenser at a flow rate of 80 kg/hr. .
  • the separated volatile components were condensed to the first condenser under the condensing condition A, and then the uncondensed volatile components were transferred to the second condenser to condense.
  • toluene is sprayed at a flow rate of 20 kg/hr to the volatile components separated from the volatilization tank and transported to the first condenser. Sprayed with hr.
  • the volatile components were separated and condensed under separation conditions and condensation conditions as described in Tables 1 to 3 below, and spray materials were sprayed on the volatile components.
  • Example 2 It was performed in the same manner as in Example 1, except that toluene was not sprayed on the volatile component separated from the volatile tank in Example 1 and being transferred to the first condenser.
  • the volatile components were separated and condensed under separation conditions and condensation conditions as described in Tables 4 to 5 below, and spray materials were sprayed on the volatile components.
  • Example 1 to 14 and Comparative Examples 1 to 16 the content of the vinyl cyan monomer not condensed in the first condenser and transferred to the second condenser is sampled in a pipe transferred from the first condenser to the second condenser, and then gas Quantitative analysis by chromatography is shown in Tables 1 to 5 below.
  • Examples 1 to 21 according to the present disclosure could be confirmed that there is no volatile component discharged without being condensed from the second condenser, so it is confirmed that the wastewater treatment cost is not required to treat it.
  • Comparative Examples 1, 8 and 12 according to the conventional method a large amount of volatile components not condensed from the second condenser was discharged at 14.8 to 58.0 kg/hr.

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Abstract

The present disclosure pertains to a manufacturing method and device for an aromatic vinyl compound-vinyl cyanide compound polymer and, more particularly, to a method for manufacturing an aromatic vinyl compound-vinyl cyanide compound polymer, the method comprising the steps of: separating a volatile component from a polymer product containing an aromatic vinyl compound-vinyl cyanide compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyanide monomer, and an organic solvent by means of a volatilization tank; and condensing the separated volatile component by means of a condenser, wherein an organic solvent or an aromatic vinyl monomer is sprayed to the volatile component being delivered to the condenser. According to the present disclosure, there are no volatile components discharged following condensation because the volatile components are entirely condensed in the condenser, whereby a reduction is brought about in a waste water treatment cost for treating the volatile components and in the air emission of vinyl cyanide monomers toxic to the human body.

Description

방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법 및 제조장치Method for manufacturing aromatic vinyl compound-vinyl cyan compound polymer and manufacturing apparatus
〔출원(들)과의 상호 인용〕(Mutual Citation with Application(s))
본 출원은 2018년 12월 18일자 한국특허출원 제10-2018-0164399호 및 이를 2019년 06월 19일자로 재출원된 한국특허출원 제10-2019-0072784호에 기초한 우선권의 이익을 주장하며, 해당 한국 특허 출원의 문헌에 개시된 모든 내용은 본 명세서의 일부로서 포함된다.This application claims the benefit of priority based on Korean Patent Application No. 10-2018-0164399 filed on December 18, 2018 and Korean Patent Application No. 10-2019-0072784 filed again on June 19, 2019, All contents disclosed in the documents of the Korean patent application are included as part of the present specification.
본 발명은 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법 및 제조장치에 관한 것으로, 보다 상세하게는 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체, 잔류 비닐시안 단량체 및 유기 용매를 포함하는 중합 생성물을 휘발조를 이용하여 휘발성 성분을 분리하는 단계; 및 분리된 휘발성 성분을 1개 또는 직렬로 연결된 2개 이상의 응축기를 이용하여 응축하는 단계;를 포함하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법으로서, 상기 휘발조에서 분리되어 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계; 또는 상기 직렬로 연결된 2개 이상의 응축기를 이용할 때 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계;를 포함하여 잔류 단량체 및 유기 용매를 저감하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법 및 제조장치에 관한 것이다.The present invention relates to a method and an apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer, and more specifically, polymerization comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent. Separating volatile components from the product using a volatilization tank; And condensing the separated volatile components using one or two or more condensers connected in series. A method for producing an aromatic vinyl compound-vinyl cyan compound polymer comprising: volatile being separated from the volatilization tank and being transferred to a condenser Spraying an organic solvent over the ingredients; Or spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser when using two or more condensers connected in series; including reducing residual monomers and organic solvents. A method for producing an aromatic vinyl compound-vinyl cyan compound polymer and a manufacturing apparatus.
일반적으로, 방향족 비닐 화합물-비닐시안 화합물 중합체는 성형성, 강성 및 전기적 특성이 우수하여 컴퓨터, 프린터, 복사기 등의 OA 기기, 텔레비전, 오디오 등의 가전 제품, 전기전자 부품, 잡화 등을 포함한 다양한 산업 분야에서 광범위하게 사용되고 있다. 특히, 내열도를 높여 외부의 높은 온도에서도 잘 견디는 방향족 비닐 화합물-비닐시안 화합물 중합체는 가전제품 하우징용, 자동차 내장재 등의 특별한 용도로 사용되고 있다.In general, the aromatic vinyl compound-vinyl cyan compound polymer has excellent moldability, stiffness, and electrical properties, and various industries including OA devices such as computers, printers, copiers, home appliances such as televisions, audio, electrical and electronic components, and miscellaneous goods. Widely used in the field. Particularly, the aromatic vinyl compound-vinyl cyan compound polymer that increases heat resistance and withstands high external temperatures is used for special purposes such as for home appliance housings and automobile interior materials.
방향족 비닐 화합물-비닐시안 화합물 중합체는 방향족 비닐 화합물 및 비닐시안 화합물을 유기 용매 하에서 반응시켜 얻어지며, 이 때 반응 후 생성되는 중합 생성물에는 방향족 비닐 화합물-비닐시안 화합물 중합체 외에 잔류 단량체 및 유기 용매가 남아 있어 이를 제거하는 공정이 필수적이다.The aromatic vinyl compound-vinyl cyan compound polymer is obtained by reacting an aromatic vinyl compound and a vinyl cyan compound under an organic solvent. At this time, residual monomers and organic solvents remain in addition to the aromatic vinyl compound-vinyl cyan compound polymer in the polymerization product produced after the reaction. Therefore, the process of removing it is essential.
반응기로부터 반응 후 배출된 중합 생성물을 휘발조로 이송하여 잔류 단량체 및 유기 용매와 같은 휘발성 성분과 방향족 비닐 화합물-비닐시안 화합물 중합체를 분리하고, 분리된 휘발성 성분은 응축기를 이용하여 응축시키고, 방향족 비닐 화합물-비닐시안 화합물 중합체는 정제 단계를 거친 후 최종 제품이 된다.After the reaction from the reactor, the discharged polymerization product is transferred to a volatilization tank to separate volatile components such as residual monomers and organic solvents from the aromatic vinyl compound-vinyl cyan compound polymer, and the separated volatile components are condensed using a condenser, and the aromatic vinyl compound -The vinyl cyan compound polymer becomes a final product after the purification step.
응축기는 일반적으로 총 2 내지 3개로 구성되며, 응축기 내의 압력이 높을수록, 냉매의 온도가 낮을수록 응축되는 양이 증가되지만, 설비 한계로 냉매의 공급 온도에 한계가 있어 응축기에서 응축되지 못한 휘발성 성분이 배출되게 된다. 또한, 끓는 점이 낮은 비닐시안 단량체가 많을수록 응축효율이 떨어진다. The condenser is generally composed of 2 to 3, and the higher the pressure in the condenser, the lower the temperature of the refrigerant increases, but the amount of condensation increases. This will be discharged. In addition, the more the vinyl cyanide monomer having a low boiling point, the lower the condensation efficiency.
응축기에서 응축되지 못한 휘발성 성분은 폐수 처리 시스템에서 처리 후 배출하거나 대기 중으로 배출하는데 이에 따른 많은 비용이 소모되고 배출된 휘발성 성분은 환경 오염 문제를 야기한다.Volatile components that are not condensed in the condenser are discharged after treatment in a wastewater treatment system or discharged to the atmosphere, and accordingly, a high cost is consumed and the volatile components discharged cause environmental pollution problems.
따라서, 응축기에서 응축 효율을 증가시켜 대기로 배출시키거나 폐수 처리 시스템으로 유입되는 휘발성 성분을 감소시키는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법의 개발이 필요한 실정이다.Accordingly, there is a need to develop a method for producing an aromatic vinyl compound-vinyl cyan compound polymer that increases condensation efficiency in a condenser and discharges it to the atmosphere or reduces volatile components introduced into a wastewater treatment system.
〔선행기술문헌〕〔Advanced technical literature〕
〔특허문헌〕[Patent Documents]
(특허문헌 1) 한국 공개특허 제10-2007-0073028호(Patent Document 1) Korean Patent Publication No. 10-2007-0073028
상기와 같은 종래기술의 문제점을 해결하고자, 본 기재는 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체, 잔류 비닐시안 단량체 및 유기 용매를 포함하는 중합 생성물을 휘발조를 이용하여 휘발성 성분을 분리하는 단계; 및 분리된 휘발성 성분을 1개 또는 직렬로 연결된 2개 이상의 응축기를 이용하여 응축하는 단계;를 포함하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법에 있어서, 상기 휘발조에서 분리되어 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계; 또는 상기 직렬로 연결된 2개 이상의 응축기를 이용할 때 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계;를 포함하여 잔류 단량체 및 유기 용매를 저감하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법 및 제조장치를 제공하는 것을 목적으로 한다.In order to solve the problems of the prior art as described above, the present disclosure separates volatile components using a volatilization tank for a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent. To do; And condensing the separated volatile components by using one or two or more condensers connected in series, wherein the method of producing an aromatic vinyl compound-vinyl cyan compound polymer is separated from the volatile tank and being transported to a condenser. Spraying an organic solvent onto the volatile component; Or spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser when using two or more condensers connected in series; including reducing residual monomers and organic solvents. An object of the present invention is to provide a method for producing an aromatic vinyl compound-vinyl cyan compound polymer and a manufacturing apparatus.
본 기재의 상기 목적 및 기타 목적들은 하기 설명된 본 기재에 의하여 모두 달성될 수 있다.The above and other objects of the present description can be achieved by the present description described below.
상기 목적을 달성하기 위하여, 본 기재는 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체, 잔류 비닐시안 단량체 및 유기 용매를 포함하는 중합 생성물을 휘발조를 이용하여 휘발성 성분을 분리하는 단계; 및 분리된 휘발성 성분을 1개 또는 직렬로 연결된 2개 이상의 응축기를 이용하여 응축하는 단계;를 포함하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법으로서, 상기 휘발조에서 분리되어 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계; 또는 상기 직렬로 연결된 2개 이상의 응축기를 이용할 때 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계;를 포함하는 것을 특징으로 하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법을 제공한다.In order to achieve the above object, the present invention comprises the steps of separating a volatile component using a volatilization tank for a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent; And condensing the separated volatile components using one or two or more condensers connected in series. A method for producing an aromatic vinyl compound-vinyl cyan compound polymer comprising: volatile being separated from the volatilization tank and being transferred to a condenser Spraying an organic solvent over the ingredients; Or when using two or more condensers connected in series, spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser. It provides a method for producing a vinyl cyan compound polymer.
또한, 본 기재는 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체, 잔류 비닐시안 단량체 및 유기 용매를 포함하는 중합 생성물로부터 휘발성 성분을 분리하는 휘발조; 및 상기 분리된 휘발성 성분을 응축시키는 1개 또는 직렬로 연결된 2개 이상의 응축기;를 포함하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조장치로, 상기 분리된 휘발성 성분을 응축기로 이송하는 이송배관에 유기 용매를 스프레이 하는 스프레이 배관을 포함하거나, 상기 직렬로 연결된 2개 이상의 응축기를 포함할 때 제1 응축기에서 응축되지 않은 휘발성 성분을 제2 응축기로 이송하는 이송배관에 유기 용매 또는 방향족 비닐 단량체를 스프레이 하는 스프레이 배관을 포함하는 것을 특징으로 하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조장치를 제공한다.In addition, the present disclosure is a volatilization tank for separating a volatile component from a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent; And one or more condensers connected in series to condense the separated volatile components; an apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer, comprising: organic in a transport pipe for transferring the separated volatile components to a condenser. Spraying organic solvents or aromatic vinyl monomers to a transport pipe that transports a volatile component that is not condensed from a first condenser to a second condenser when it includes a spray pipe for spraying a solvent or when two or more condensers connected in series are included. It provides an apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer comprising a spray pipe.
본 기재에 따르면, 방향족 비닐 화합물-비닐시안 화합물 중합체 제조 시 설비 교체 없이 제1 응축기로 이송 중인 휘발성 성분, 또는 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기 용매 또는 방향족 비닐 단량체를 스프레이 하여 휘발성 성분 내에 비점이 낮은 비닐시안 단량체의 함량을 낮춰 응축 효율을 향상시킴으로써 응축되지 않은 휘발성 성분을 처리하기 위한 폐수 처리 비용이 저감되고 인체에 해로운 휘발성 성분이 대기 중으로 배출되는 양이 현저하게 감소되는 효과가 있다.According to the present description, in the manufacture of the aromatic vinyl compound-vinyl cyan compound polymer, an organic solvent or aromatic vinyl monomer is added to the volatile component being transferred to the first condenser without replacement of the equipment, or to the volatile component not being condensed from the first condenser and being transferred to the second condenser. By spraying, it lowers the content of vinyl cyanide monomer having a low boiling point in the volatile component to improve the condensation efficiency, thereby reducing the cost of wastewater treatment to treat volatile components that are not condensed and the amount of volatile components harmful to the human body discharged to the atmosphere is remarkable. It has a decreasing effect.
도 1은 본 기재에 따른 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체 및 유기 용매를 포함하는 중합 생성물로부터 휘발성 성분을 분리 및 응축하는 단계를 개략적으로 도시한 도면이다.1 is a view schematically showing a step of separating and condensing volatile components from a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, residual aromatic vinyl monomer and an organic solvent according to the present disclosure.
도 2는 종래 기술에 따른 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체 및 유기 용매를 포함하는 중합 생성물로부터 휘발성 성분을 분리 및 응축하는 단계를 개략적으로 도시한 도면이다.2 is a view schematically showing a step of separating and condensing a volatile component from a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, residual aromatic vinyl monomer and an organic solvent according to the prior art.
이하 본 기재의 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법을 상세하게 설명한다.Hereinafter, a method for producing the aromatic vinyl compound-vinyl cyan compound polymer of the present description will be described in detail.
본 발명자들은 방향족 비닐 화합물-비닐시안 화합물 중합체를 제조하는 과정에서 중합 생성물로부터 분리된 휘발성 성분이 응축단계에서 충분히 응축되지 못하고 배출됨으로써 발생되는 폐수 처리 비용 및 환경 오염 문제를 해결하고자 부단히 노력한 결과, 응축기로 이송 중인 휘발성 성분에 유기 용매 또는 단량체를 투입함으로써, 응축 효율이 상승되어 응축되지 되지 않고 배출되는 휘발성 성분이 감소되는 효과를 확인하고, 이를 토대로 연구에 더욱 매진하여 본 발명을 완성하게 되었다.As a result of continuous efforts to solve the problem of wastewater treatment and environmental pollution caused by volatile components separated from the polymerization product not being sufficiently condensed during the condensation step in the process of preparing the aromatic vinyl compound-vinyl cyan compound polymer, the present inventors condenser By introducing an organic solvent or a monomer to the volatile component being transported to the furnace, the condensation efficiency is increased to confirm the effect that the volatile component is discharged without being condensed, and based on this, the study was further conducted to complete the present invention.
본 기재에 의한 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법을 상세하게 살펴보면 다음과 같다.Looking at the method for producing an aromatic vinyl compound-vinyl cyan compound polymer according to the present invention in detail as follows.
본 발명의 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법은 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체, 잔류 비닐시안 단량체 및 유기 용매를 포함하는 중합 생성물을 휘발조를 이용하여 휘발성 성분을 분리하는 단계; 및 분리된 휘발성 성분을 1개 또는 직렬로 연결된 2개 이상의 응축기를 이용하여 응축하는 단계;를 포함하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법으로서, 상기 휘발조에서 분리되어 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계; 또는 상기 직렬로 연결된 2개 이상의 응축기를 이용할 때 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계;를 포함하는 것을 특징으로 하고, 이 경우에 응축효율이 높아져서 배출되는 휘발성 성분이 현저히 감소되는 효과가 있다.In the method for producing an aromatic vinyl compound-vinyl cyan compound polymer of the present invention, a volatile component of a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent is volatilized. Separating; And condensing the separated volatile components using one or two or more condensers connected in series. A method for producing an aromatic vinyl compound-vinyl cyan compound polymer comprising: volatile being separated from the volatilization tank and being transferred to a condenser Spraying an organic solvent over the ingredients; Or when using two or more condensers connected in series, spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser. The condensation efficiency is increased, and the volatile components discharged are significantly reduced.
본 기재에서 제1 응축기와 제2 응축기는 직렬로 연결된 2개 이상의 응축기 중 임의의 두 개의 응축기 사이에서 전 단계의 응축기와 후 단계의 응축기를 의미한다.In the present description, the first condenser and the second condenser mean a condenser of a previous stage and a condenser of a later stage between any two condensers of two or more condensers connected in series.
일례로, 본 기재의 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법은 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체, 잔류 비닐시안 단량체 및 유기 용매를 포함하는 중합 생성물을 휘발조를 이용하여 휘발성 성분을 분리하는 단계; 및 분리된 휘발성 성분을 직렬로 연결된 2개 이상의 응축기를 이용하여 응축하는 단계;를 포함하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법에 있어서, 상기 휘발조에서 분리되어 제1 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계; 또는 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계;를 포함하는 것을 특징으로 하고, 이 경우에 응축효율이 높아져서 배출되는 휘발성 성분이 현저히 감소되는 효과가 있다.In one example, the method for producing an aromatic vinyl compound-vinyl cyan compound polymer of the present disclosure uses a volatilization tank for a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent. Separating volatile components; And condensing the separated volatile components using two or more condensers connected in series. A method for producing an aromatic vinyl compound-vinyl cyan compound polymer comprising: volatile being separated from the volatilization tank and being transported to a first condenser. Spraying an organic solvent over the ingredients; Or spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser, and in this case, the condensation efficiency is increased to significantly reduce the volatile components discharged. It has an effect.
상기 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법은, 일례로 상기 휘발조에서 분리되어 제1 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계; 및 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계;를 포함할 수 있고, 이 경우에 응축효율이 높아져서 배출되는 휘발성 성분이 현저히 감소되는 효과가 있다.The method for producing the aromatic vinyl compound-vinyl cyan compound polymer includes, for example, spraying an organic solvent to a volatile component separated from the volatile tank and being transferred to a first condenser; And spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not being condensed in the first condenser and is being transferred to the second condenser; in this case, the condensation efficiency is increased and the volatile component discharged is significantly reduced. There is.
일례로 상기 휘발성 성분을 분리하는 단계 이전에 방향족 비닐 화합물과 비닐시안 화합물을 중합 반응시키는 단계가 포함될 수 있다.For example, a step of polymerizing the aromatic vinyl compound and the vinyl cyan compound before the step of separating the volatile components may be included.
상기 방향족 비닐 화합물-비닐시안 화합물 중합체는 일례로 방향족 비닐 화합물 및 비닐시안 화합물을 유기 용매 하에서 반응시켜 제조할 수 있다.The aromatic vinyl compound-vinyl cyan compound polymer may be prepared, for example, by reacting an aromatic vinyl compound and a vinyl cyan compound under an organic solvent.
상기 중합 반응은 일례로 개시제, 분자량 조절제 및 유화제로 이루어진 군으로부터 선택된 1종 이상을 포함하여 반응시킬 수 있다.The polymerization reaction may include, for example, one or more selected from the group consisting of an initiator, a molecular weight modifier, and an emulsifier.
상기 반응은 일례로 괴상 중합법, 용액 중합법 또는 유화 중합법일 수 있고 바람직하게는 괴상 중합법 또는 용액 중합법일 수 있으며, 이 경우에 제조된 방향족 비닐 화합물-비닐시안 화합물 중합체의 인장강도, 충격강도 등의 기계적 물성과 내열성, 열안정성이 우수한 효과가 있다.The reaction may be, for example, a bulk polymerization method, a solution polymerization method or an emulsion polymerization method, preferably a bulk polymerization method or a solution polymerization method, and in this case, the tensile strength and impact strength of the aromatic vinyl compound-vinyl cyan compound polymer prepared in this case. It has excellent mechanical properties, heat resistance, and thermal stability.
본 발명에서 방향족 비닐 화합물-비닐시안 화합물 중합체를 수득하기 위한 반응시키는 방법은 특별히 제한되지 않고, 일반적으로 사용되는 중합 방법이 사용될 수 있다.In the present invention, a method for reacting to obtain an aromatic vinyl compound-vinyl cyan compound polymer is not particularly limited, and a commonly used polymerization method can be used.
상기 휘발조에서 휘발성 성분을 분리하는 단계는 일례로 220 내지 260℃ 및 35 torr 이하, 바람직하게는 225 내지 255℃ 및 15 내지 35 torr의 조건 하에서 수행될 수 있고, 이 범위 내에서 휘발성 성분과 방향족 비닐 화합물-비닐시안 화합물 중합체의 분리가 원활히 수행되는 효과가 있다.The step of separating volatile components from the volatilization tank may be performed under the conditions of 220 to 260°C and 35 torr or less, preferably 225 to 255°C and 15 to 35 torr, for example, and within this range, volatile components and aromatics There is an effect that the separation of the vinyl compound-vinyl cyan compound polymer is smoothly performed.
본 기재에서 휘발조는 본 발명이 속한 기술분야에서 일반적으로 사용되는 휘발조인 경우 특별히 제한되지 않고 일반적으로 적용되는 휘발조가 사용될 수 있다.In the present description, the volatile tank is not particularly limited when the volatile tank is generally used in the technical field to which the present invention belongs, and a volatile tank that is generally applied may be used.
상기 분리된 휘발성 성분은 일례로 비닐시안 화합물 5 내지 35 중량%, 방향족 비닐 화합물 45 내지 80 중량% 및 유기 용매 5 내지 50 중량%를 포함할 수 있다.The separated volatile component may include, for example, 5 to 35% by weight of a vinyl cyan compound, 45 to 80% by weight of an aromatic vinyl compound, and 5 to 50% by weight of an organic solvent.
구체적인 예로, 상기 분리된 휘발성 성분은 비닐시안 화합물 5 내지 20 중량%, 방향족 비닐 화합물 45 내지 59 중량% 및 유기 용매 25 내지 45 중량%를 포함하거나, 비닐시안 화합물 15 내지 35 중량%, 방향족 비닐 화합물 60 내지 80 중량% 및 유기 용매 5 내지 25 중량%를 포함할 수 있다.As a specific example, the separated volatile component contains 5 to 20% by weight of a vinyl cyan compound, 45 to 59% by weight of an aromatic vinyl compound and 25 to 45% by weight of an organic solvent, or 15 to 35% by weight of a vinyl cyan compound, an aromatic vinyl compound 60 to 80% by weight and 5 to 25% by weight of an organic solvent.
상기 휘발조를 통과한 방향족 비닐 화합물-비닐시안 화합물 중합체는 일례로 펠리타이저(pelletizer)로 이송되어 절단된 후 냉각 및 건조하여 펠릿(pellet)으로 수득할 수 있다.The aromatic vinyl compound-vinyl cyan compound polymer that has passed through the volatilization tank may be, for example, transferred to a pelletizer, cut, cooled and dried to obtain pellets.
상기 응축기는 바람직하게는 2개 이상의 응축기가 직렬로 연결되거나 또는 2개의 응축기가 직렬로 연결될 수 있고, 이 경우에 응축 효율이 증가되는 효과가 있다.The condenser is preferably two or more condensers connected in series or two condensers can be connected in series, in this case there is an effect that the condensing efficiency is increased.
본 기재에서 응축기는 본 발명이 속한 기술분야에서 일반적으로 사용되는 응축기인 경우 특별히 제한되지 않고 일반적으로 적용되는 응축기가 사용될 수 있다.The condenser in the present description is not particularly limited when the condenser is generally used in the technical field to which the present invention belongs, and a condenser that is generally applied may be used.
상기 휘발조에서 분리되어 제1 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계는, 일례로 유기 용매를 유량 10 내지 200 kg/hr, 10 내지 150 kg/hr, 또는 15 내지 100 kg/hr, 바람직하게는 15 내지 90 kg/hr, 보다 바람직하게는 20 내지 50 kg/hr로 스프레이 할 수 있고, 이 경우에 휘발성 성분 내에 비점이 낮은 잔류 비닐시안 단량체의 함량비가 감소되어 응축 효율이 증대되는 효과가 있다.The step of spraying the organic solvent to the volatile components separated from the volatilization tank and being transported to the first condenser is, for example, an organic solvent flow rate of 10 to 200 kg/hr, 10 to 150 kg/hr, or 15 to 100 kg/hr , Preferably it can be sprayed at 15 to 90 kg/hr, more preferably 20 to 50 kg/hr, and in this case, the content ratio of the residual vinyl cyan monomer having a low boiling point in the volatile component is reduced to increase condensation efficiency. It works.
상기 휘발조에서 분리되어 제1 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계; 및 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계는, 일례로 제1 응축기로 이송 중인 휘발성 성분에 유기 용매를 10 내지 100 kg/hr, 바람직하게는 20 내지 90 kg/hr로 스프레이 할 수 있고, 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 10 내지 100 kg/hr, 바람직하게는 15 내지 90 kg/hr로 스프레이 할 수 있고, 이 경우에 응축효율이 높아져서 배출되는 휘발성 성분이 현저히 감소되는 효과가 있다.Spraying an organic solvent to a volatile component separated from the volatilization tank and being transported to a first condenser; And spraying the organic solvent or aromatic vinyl monomer to the volatile component that is not condensed in the first condenser and is being transferred to the second condenser, for example, 10 to 100 kg/hr of an organic solvent to the volatile component that is being transferred to the first condenser, Preferably, it can be sprayed at 20 to 90 kg/hr, and 10 to 100 kg/hr, preferably 15 to 15, of organic solvent or aromatic vinyl monomer is added to the volatile component that is not condensed in the first condenser and is being transferred to the second condenser. It can be sprayed at 90 kg/hr, and in this case, the condensation efficiency is increased, so that the volatile components discharged are significantly reduced.
상기 휘발조에서 분리되어 제1 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계는, 일례로 유기 용매를 온도 -10℃ 내지 40℃, 바람직하게는 0 내지 30℃, 보다 바람직하게는 15℃ 내지 25℃ 범위로 스프레이 할 수 있고, 이 범위 내에서 응축 효율이 증대되는 효과가 있다.The step of spraying the organic solvent to the volatile component being separated from the volatilization tank and being transported to the first condenser, for example, the temperature of the organic solvent is -10 ℃ to 40 ℃, preferably 0 to 30 ℃, more preferably 15 ℃ It can be sprayed in the range of 25 to 25 ℃, there is an effect that condensation efficiency is increased within this range.
본 발명에서 제1 응축기로 스프레이 되는 유기 용매의 온도는 특별히 한정되지 않는다.In the present invention, the temperature of the organic solvent sprayed to the first condenser is not particularly limited.
상기 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계는, 일례로 유기용매 또는 방향족 비닐 단량체를 유량 10 내지 200 kg/hr, 또는 10 내지 110 kg/hr, 바람직하게는 10 내지 90 kg/hr, 보다 바람직하게는 10 내지 40 kg/hr로 스프레이 할 수 있고, 이 경우에 휘발성 성분 내에 비점이 낮은 잔류 비닐시안 단량체의 함량비가 감소되어 응축 효율이 증대되는 효과가 있다.The step of spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser is, for example, an organic solvent or an aromatic vinyl monomer flow rate of 10 to 200 kg/hr, or 10 to 110 It can be sprayed at kg/hr, preferably 10 to 90 kg/hr, more preferably 10 to 40 kg/hr, and in this case, the content ratio of the residual vinyl cyan monomer having a low boiling point in the volatile component is reduced, thereby condensing efficiency. This increases the effect.
본 기재에서 유량은 유량계로 측정하거나 물질수지(mass balance) 식으로 계산할 수 있다. 상기 물질수지(mass balance) 식으로 미응축 유량은 투입량-생산량-회수량으로 계산될 수 있다.In the present description, the flow rate can be measured by a flow meter or calculated by mass balance. The non-condensed flow rate may be calculated as an input amount-production amount-recovery amount using the mass balance formula.
상기 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계는, 일례로 유기용매 또는 방향족 비닐 단량체를 온도 -10℃ 내지 40℃, 바람직하게는 0℃ 내지 30℃, 보다 바람직하게는 15℃ 내지 25℃ 범위 내로 스프레이 할 수 있고, 이 범위 내에서 응축 효율이 증대되는 효과가 있다.The step of spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and being transported to the second condenser is, for example, an organic solvent or an aromatic vinyl monomer temperature -10 ℃ to 40 ℃, preferably 0 ℃ to 30 ℃, more preferably can be sprayed in the range of 15 ℃ to 25 ℃, there is an effect that increases the condensing efficiency within this range.
본 발명에서 제2 응축기로 스프레이 되는 유기 용매 또는 방향족 비닐 단량체의 온도는 특별히 한정되지 않는다. In the present invention, the temperature of the organic solvent or aromatic vinyl monomer sprayed to the second condenser is not particularly limited.
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상기 제1 응축기에서 응축은 일례로 냉매 온도 20℃ 내지 35℃ 및 운전압력 3 내지 100 torr 조건, 바람직하게는 냉매 온도 25℃ 내지 33℃ 및 운전압력 15 내지 35 torr 조건, 보다 바람직하게는 냉매 온도 25℃ 내지 30℃ 및 운전압력 15 내지 30 torr 조건 하에서 수행될 수 있고, 이 범위 내에서 응축 효율이 증가하는 효과가 있다.The condensation in the first condenser is, for example, a refrigerant temperature of 20°C to 35°C and an operating pressure of 3 to 100 torr, preferably a refrigerant temperature of 25°C to 33°C and an operating pressure of 15 to 35 torr, more preferably of a refrigerant temperature. 25 ℃ to 30 ℃ and can be carried out under the operating pressure of 15 to 30 torr conditions, there is an effect of increasing the condensation efficiency within this range.
본 기재에서 응축기의 운전압력은 응축기를 운전할 때 걸리는 응축기 내압을 의미한다.In this description, the operating pressure of the condenser means the internal pressure of the condenser applied when operating the condenser.
상기 제2 응축기에서 응축은 일례로 냉매 온도는 -3℃ 내지 4℃ 및 운전압력 5 내지 50 torr 조건, 바람직하게는 냉매 온도는 -1℃ 내지 4℃ 및 운전압력 7 내지 25 torr 조건, 보다 바람직하게는 냉매 온도는 0℃ 내지 4℃ 및 운전압력 10 내지 20 torr 조건 하에서 수행될 수 있고, 이 범위 내에서 응축 효율이 증가하는 효과가 있다.Condensation in the second condenser is, for example, the refrigerant temperature is -3 ℃ to 4 ℃ and the operating pressure 5 to 50 torr condition, preferably the refrigerant temperature is -1 ℃ to 4 ℃ and the operating pressure 7 to 25 torr condition, more preferably For example, the refrigerant temperature may be performed under conditions of 0°C to 4°C and an operating pressure of 10 to 20 torr, and there is an effect of increasing condensation efficiency within this range.
상기 제1 응축기 및 제2 응축기로부터 응축된 응축물은 일례로 회수 및 정제되어 반응기로 재투입될 수 있고, 이 경우에 원료비가 절감되는 효과가 있다.The condensate condensed from the first condenser and the second condenser can be recovered and purified, for example, and re-entered into the reactor, and in this case, the raw material cost is reduced.
상기 제2 응축기에서 응축되지 않는 휘발성 성분은 일례로 진공 유닛(vacuum unit)으로 이송되어 수냉식 펌프의 순환액에 용해되어 폐수처리 단계를 거친 후 배출되며, 이 과정에서 일부는 대기로 방출될 수 있고, 이 경우에 대기로 방출되는 휘발성 성분이 현저히 감소되어 환경 오염을 방지하는 효과가 있다.Volatile components that are not condensed in the second condenser are transferred to a vacuum unit, for example, dissolved in a circulating fluid of a water-cooled pump and discharged after a wastewater treatment step, and in this process, some may be released into the atmosphere. In this case, in this case, the volatile components released into the atmosphere are significantly reduced, thereby preventing environmental pollution.
상기 유기 용매는 일례로 톨루엔, 에틸 벤젠, 자일렌, 메틸에틸케톤 및 메틸이소부틸케톤으로 이루어진 군으로부터 선택된 1종 이상일 수 있고, 바람직하게는 상기 중합 반응에서 사용되는 유기 용매와 상기 스프레이 되는 유기 용매가 동일한 것이며, 이 경우에 휘발성 성분 내에 비점이 높은 성분이 추가됨으로써 비점이 낮은 성분, 즉 잔류 비닐시안 단량체의 함량비가 낮아져 응축효율이 향상되는 효과가 있다.The organic solvent may be, for example, one or more selected from the group consisting of toluene, ethyl benzene, xylene, methyl ethyl ketone and methyl isobutyl ketone, preferably the organic solvent used in the polymerization reaction and the organic solvent sprayed Is the same, and in this case, by adding a component having a high boiling point in the volatile component, the content ratio of the component having a low boiling point, that is, the residual vinyl cyan monomer is lowered, thereby improving condensation efficiency.
상기 방향족 비닐 화합물은 일례로 스티렌, α-메틸 스티렌, p-메틸 스티렌, p-브로모스티렌, p-클로로스티렌 및 o-브로모스티렌으로 이루어진 군으로부터 선택된 1종 이상일 수 있고, 이 경우에 휘발성 성분 내에 비점이 낮은 잔류 비닐시안 단량체의 함량비를 낮춰 응축효율이 향상되는 효과가 있다.The aromatic vinyl compound may be, for example, one or more selected from the group consisting of styrene, α-methyl styrene, p-methyl styrene, p-bromostyrene, p-chlorostyrene and o-bromostyrene, in this case volatile There is an effect that the condensation efficiency is improved by lowering the content ratio of the residual vinyl cyan monomer in the component having a low boiling point.
본 발명의 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조장치는 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체, 잔류 비닐시안 단량체 및 유기 용매를 포함하는 중합 생성물로부터 휘발성 성분을 분리하는 휘발조; 및 상기 분리된 휘발성 성분을 응축시키는 1개 또는 직렬로 연결된 2개 이상의 응축기;를 포함하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조장치로, 상기 분리된 휘발성 성분을 응축기로 이송하는 이송배관에 유기 용매를 스프레이 하는 스프레이 수단을 포함하거나, 상기 직렬로 연결된 2개 이상의 응축기를 포함할 때 제1 응축기에서 응축되지 않은 휘발성 성분을 제2 응축기로 이송하는 이송배관에 유기 용매 또는 방향족 비닐 단량체를 스프레이 하는 스프레이 수단을 포함하는 것을 특징으로 하고, 이 경우에 응축효율이 향상되어 응축 후 배출되는 휘발성 성분이 거의 존재하지 않는 효과가 있다.The apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer of the present invention includes a volatilization tank for separating volatile components from a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, residual aromatic vinyl monomer, residual vinyl cyan monomer and organic solvent; And one or more condensers connected in series to condense the separated volatile components; an apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer, comprising: organic in a transport pipe for transferring the separated volatile components to a condenser. Spraying means for spraying a solvent, or spraying an organic solvent or an aromatic vinyl monomer to a transfer pipe that transports volatile components that are not condensed from the first condenser to the second condenser when including two or more condensers connected in series. It characterized in that it comprises a spray means, in this case, the condensation efficiency is improved, there is an effect that almost no volatile components are discharged after condensation.
본 기재에서 스프레이 수단은 이송 배관에 연결되어 이송 배관 내부로 유기 용매 또는 방향족 비닐 단량체를 분무할 수 있는 수단인 경우 특별히 제한되지 않고, 일례로 스프레이 배관, 스프레이 용기 등일 수 있으며, 스프레이 노즐을 포함할 수 있다.In the present description, the spray means is not particularly limited in the case of a means capable of spraying an organic solvent or an aromatic vinyl monomer into the transfer pipe and connected to the transfer pipe, and may be, for example, a spray pipe, a spray container, or the like, and include a spray nozzle. Can.
일례로, 본 기재의 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조장치는 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체, 잔류 비닐시안 단량체 및 유기 용매를 포함하는 중합 생성물로부터 휘발성 성분을 분리하는 휘발조; 및 상기 분리된 휘발성 성분을 응축시키는 직렬로 연결된 2개 이상의 응축기;를 포함하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조장치로, 상기 분리된 휘발성 성분을 제1 응축기로 이송하는 이송배관에 유기 용매를 스프레이 하는 스프레이 배관을 포함하거나, 제1 응축기에서 응축되지 않은 휘발성 성분을 제2 응축기로 이송하는 이송배관에 유기 용매 또는 방향족 비닐 단량체를 스프레이 하는 스프레이 배관을 포함하는 것을 특징으로 하고, 이 경우에 응축효율이 향상되어 응축 후 배출되는 휘발성 성분이 거의 존재하지 않는 효과가 있다.In one example, the apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer of the present disclosure separates volatile components from a polymerization product including an aromatic vinyl compound-vinyl cyan compound polymer, residual aromatic vinyl monomer, residual vinyl cyan monomer, and organic solvent. Volatilization; And two or more condensers connected in series to condense the separated volatile components. An aromatic vinyl compound-vinyl cyan compound polymer manufacturing apparatus comprising: an organic solvent in a transport pipe for transferring the separated volatile components to a first condenser. It characterized in that it comprises a spray pipe for spraying an organic solvent or an aromatic vinyl monomer to the transfer pipe for transporting a volatile component that is not condensed in the first condenser to the second condenser, or in this case, Condensation efficiency is improved so that there is almost no volatile component discharged after condensation.
상기 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조장치는 일례로 상기 분리된 휘발성 성분을 제1 응축기로 이송하는 이송배관에 유기용매를 스프레이 하는 스프레이 배관을 포함하고, 제1 응축기에서 응축되지 않은 휘발성 성분을 제2 응축기로 이송하는 이송배관에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 스프레이 배관을 포함할 수 있고, 이 경우에 응축효율이 향상되어 제2 응축기에서 응축 후 배출되는 휘발성 성분이 거의 존재하지 않는 효과가 있다.The apparatus for manufacturing the aromatic vinyl compound-vinyl cyan compound polymer includes, for example, a spray pipe for spraying an organic solvent to a transport pipe for transporting the separated volatile component to the first condenser, and the volatile component not condensed in the first condenser It may include a spray pipe for spraying an organic solvent or an aromatic vinyl monomer in the transfer pipe to the second condenser, in which case the condensation efficiency is improved so that there is almost no volatile components discharged after condensation in the second condenser It works.
상기 스프레이 배관은 일례로 노즐을 포함할 수 있다.The spray pipe may include, for example, a nozzle.
본 발명의 노즐은 본 발명이 속한 기술분야에서 일반적으로 사용되는 노즐인 경우 특별히 제한되지 않고 일반적으로 적용되는 노즐이 사용될 수 있다.When the nozzle of the present invention is a nozzle generally used in the technical field to which the present invention belongs, it is not particularly limited and a nozzle that is generally applied may be used.
상기 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조장치에 포함된 휘발조 및 응축기 등은 상술된 내용을 따르므로 그 기재를 생략한다.Volatile tanks, condensers, and the like included in the aromatic vinyl compound-vinyl cyan compound polymer manufacturing apparatus follow the above description, and the description thereof will be omitted.
본 발명에 따른 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법 및 제조장치를 하기 도 1 및 2를 참조하여 설명한다. 이러한 도면은 단지 본 발명을 예시하는 개략도일 뿐 묘사된 실시 태양에 제한되지 않으며, 이해가 쉽도록 본 발명을 설명하기 위해 필요한 수단만을 묘사하였으며, 방법 및 장치를 수행하기 위해 필요한 다른 자명한 수단은 도면에서 생략하였다.A method and an apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer according to the present invention will be described with reference to FIGS. 1 and 2 below. These drawings are only schematic diagrams illustrating the present invention and are not limited to the depicted embodiments, and merely depict the means necessary to describe the present invention for ease of understanding, and other obvious means necessary to perform the methods and apparatus are Omitted from the drawings.
하기 도 1은 본 발명에 따른 실시예 1 내지 21에 사용된 휘발조(DV), 제1 응축기(1st CN), 제2 응축기(2nd CN), 진공 유닛(Vacuum Unit), 이송배관 및 스프레이 배관을 개략적으로 도시한 도면으로, 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체, 잔류 비닐 시안 단량체 및 유기 용매를 포함하는 중합 생성물을 휘발조에서 휘발성 성분을 분리하고, 분리된 휘발성 성분을 제1 응축기로 이송하는 이송배관에 스프레이 배관을 통해 유기 용매를 스프레이 하거나, 제1 응축기에서 응축되지 않은 휘발성 성분을 제2 응축기로 이송하는 이송배관에 유기 용매 또는 방향족 비닐 단량체를 스프레이 배관을 통해 스프레이 하는 것을 포함하는 제조장치를 나타낸 것이다. 1 is a volatilization tank (DV), a first condenser (1 st CN), a second condenser (2 nd CN), a vacuum unit, a transport piping used in Examples 1 to 21 according to the present invention, and As a schematic drawing of a spray pipe, a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent is separated from a volatile component in a volatilization tank, and the separated volatile component Spray the organic solvent through the spray pipe to the transfer pipe to the first condenser, or organic solvent or aromatic vinyl monomer to the transfer pipe to transfer the volatile components not condensed from the first condenser to the second condenser through the spray pipe It shows a manufacturing apparatus including spraying.
또한, 제2 응축기에서 응축되지 않은 휘발성 성분을 진공 유닛으로 이송하여 수냉식 펌프의 순환액에 용해시켜 폐수처리하여 배출하거나 대기로 배출시킨다.In addition, the volatile components that are not condensed in the second condenser are transferred to a vacuum unit, dissolved in the circulating fluid of the water-cooled pump, discharged by treatment with waste water or discharged to the atmosphere.
상기 도면에 나타내지는 않았으나, 제1 응축기 및 제2 응축기로부터 응축된 응축물은 반응기로 재투입될 수 있다.Although not shown in the figure, condensate condensed from the first condenser and the second condenser may be re-entered into the reactor.
또한, 하기 도 2는 비교예 1, 8 및 12에 사용된 휘발조(DV), 제1 응축기(1st CN), 제2 응축기(2nd CN) 및 진공 유닛(Vacuum Unit)을 개략적으로 도시한 도면으로, 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체 및 유기 용매를 포함하는 중합 생성물은 휘발조에서 휘발성 성분이 분리되어 제1 응축기 및 제2 응축기를 거쳐 응축되고, 제2 응축기에서 응축되지 않은 휘발성 성분은 진공 유닛으로 이송되어 펌프를 통해 압축되고 수냉식 펌프의 순환액에 용해되어 폐수 처리되어 배출되거나 대기로 배출된다.In addition, Figure 2 below schematically shows the volatile tank (DV), the first condenser (1 st CN), the second condenser (2 nd CN) and the vacuum unit (Vacuum Unit) used in Comparative Examples 1, 8 and 12 In one drawing, a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, and an organic solvent is separated from a volatile component in a volatilization tank and condensed through a first condenser and a second condenser, and in a second condenser The non-condensed volatile components are transferred to a vacuum unit, compressed through a pump, dissolved in a circulating fluid of a water-cooled pump, treated as wastewater, and discharged or discharged to the atmosphere.
상기 도면에 나타내지는 않았으나, 제1 응축기 및 제2 응축기에서 응축된 응축물은 반응기로 재투입될 수 있다.Although not shown in the figure, the condensate condensed in the first condenser and the second condenser may be re-entered into the reactor.
이하, 본 기재의 이해를 돕기 위하여 바람직한 실시예를 제시하나, 하기 실시예는 본 기재를 예시하는 것일 뿐 본 기재의 범주 및 기술사상 범위 내에서 다양한 변경 및 수정이 가능함은 당업자에게 있어서 명백한 것이며, 이러한 변형 및 수정이 첨부된 특허청구범위에 속하는 것도 당연한 것이다.Hereinafter, a preferred embodiment is provided to help understanding of the present description, but the following examples are merely illustrative of the present description, and it is apparent to those skilled in the art that various changes and modifications are possible within the scope and technical thought scope of the present description, It is no wonder that such variations and modifications fall within the scope of the appended claims.
[실시예][Example]
하기 표 1 내지 5에서 각 단계별 조건은 다음과 같다.The conditions for each step in Tables 1 to 5 are as follows.
휘발성 성분을 분리하는 단계Separating volatile components
* 분리조건 A: 온도 230℃, 압력 20 torr의 조건 하에서 수행되고, 이 때 휘발조에서 분리된 휘발성 성분은 스티렌 단량체 55.8 중량%, 아크릴로니트릴 단량체 7.25 중량% 및 톨루엔 37 중량%를 포함하였다.* Separation conditions A: temperature 230 ℃, the pressure was carried out under the conditions of 20 torr, at this time, the volatile components separated from the volatile bath included 55.8% by weight of styrene monomer, 7.25% by weight of acrylonitrile monomer and 37% by weight of toluene.
* 분리조건 B: 온도 250℃, 압력 30 torr의 조건 하에서 수행되고, 이 때 휘발조에서 분리된 휘발성 성분은 스티렌 단량체 68.2 중량%, 아크릴로니트릴 단량체 23.7 중량% 및 톨루엔 9.1 중량%를 포함하였다.* Separation condition B: temperature 250 ℃, pressure was performed under the conditions of 30 torr, at this time, the volatile components separated from the volatilization tank included 68.2% by weight of styrene monomer, 23.7% by weight of acrylonitrile monomer and 9.1% by weight of toluene.
* 분리조건 C: 온도 240℃, 압력 20 torr의 조건 하에서 수행되고, 이 때 휘발조에서 분리된 휘발성 성분은 스티렌 단량체 62 중량%, 아크릴로니트릴 단량체 15 중량% 및 톨루엔 23 중량%를 포함하였다.* Separation conditions C: temperature 240 ℃, the pressure was carried out under the conditions of 20 torr, at this time, the volatile components separated from the volatilization tank included 62% by weight of styrene monomer, 15% by weight of acrylonitrile monomer and 23% by weight of toluene.
응축 단계Condensation step
* 응축조건 A: 제1 응축기는 냉매 온도 30℃, 압력 20 torr의 조건 하에서, 제2 응축기는 냉매 온도 2℃, 압력 10 torr 하에서 수행하였다.* Condensation condition A: The first condenser was performed under the condition of the refrigerant temperature of 30°C and the pressure of 20 torr, and the second condenser was performed under the refrigerant temperature of 2°C and the pressure of 10 torr.
* 응축조건 B: 제1 응축기는 냉매 온도 30℃, 압력 30 torr의 조건 하에서, 제2 응축기는 냉매 온도 2℃, 압력 20 torr의 조건 하에서 수행하였다.* Condensation condition B: The first condenser was performed under the condition of the refrigerant temperature of 30°C and the pressure of 30 torr, and the second condenser was performed under the condition of the refrigerant temperature of 2°C and the pressure of 20 torr.
* 응축조건 C: 제1 응축기는 냉매 온도 25℃, 압력 15 torr의 조건 하에서, 제2 응축기는 냉매 온도 -1℃, 압력 10 torr 하에서 수행하였다.* Condensation condition C: The first condenser was performed under the condition of a refrigerant temperature of 25°C and a pressure of 15 torr, and the second condenser was performed under a refrigerant temperature of -1°C and a pressure of 10 torr.
* 스프레이 물질: 톨루엔은 "1"로 표시, 스티렌은 "2"로 표시, α-메틸 스티렌은 "3"으로 표시, 아크릴로니트릴은 "4"로 표시, 및 메타크릴로니트릴은 "5"로 표시하였다. * Spray material: toluene indicated as "1", styrene indicated as "2", α-methyl styrene indicated as "3", acrylonitrile indicated as "4", and methacrylonitrile marked as "5" It was denoted as.
실시예 1Example 1
분리조건 A 하에서 휘발성 성분을 분리한 다음, 분리된 휘발성 성분을 응축조건 A 하에서 제1 응축기로 응축 후 응축되지 않은 휘발성 성분을 제2 응축기로 이송하여 응축하였다. 이 때, 휘발조에서 분리되어 제1 응축기로 이송 중인 휘발성 성분에 톨루엔을 유량 45 kg/hr로 스프레이 하고, 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에는 스프레이 하지 않았다.After separating the volatile components under the separation condition A, the separated volatile components were condensed to the first condenser under the condensation condition A, and then the uncondensed volatile components were transferred to the second condenser and condensed. At this time, toluene was sprayed at a flow rate of 45 kg/hr to the volatile components separated from the volatile tank and being transported to the first condenser, and volatile components not condensed in the first condenser and being transported to the second condenser were not sprayed.
실시예 2Example 2
분리조건 A 하에서 휘발성 성분을 분리한 다음, 분리된 휘발성 성분을 응축조건 A 하에서 제1 응축기로 응축 후 응축되지 않은 휘발성 성분을 제2 응축기로 이송하여 응축하였다. 이 때, 휘발조에서 분리된 휘발성 성분을 제1 응축기로 이송 중인 휘발성 성분에는 스프레이 하지 않고, 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 스티렌을 유량 30 kg/hr로 스프레이 하였다. After separating the volatile components under the separation condition A, the separated volatile components were condensed to the first condenser under the condensation condition A, and then the uncondensed volatile components were transferred to the second condenser and condensed. At this time, the volatile components separated from the volatile tank were not sprayed on the volatile components being transferred to the first condenser, and styrene was sprayed on the volatile components not being condensed on the first condenser and being transferred to the second condenser at a flow rate of 30 kg/hr. .
실시예 3Example 3
분리조건 A 하에서 휘발성 성분을 분리한 다음, 분리된 휘발성 성분을 응축조건 A 하에서 제1 응축기로 응축 후 응축되지 않은 휘발성 성분을 제2 응축기로 이송하여 응축하였다. 이 때, 휘발조에서 분리된 휘발성 성분을 제1 응축기로 이송 중인 휘발성 성분에는 스프레이 하지 않고, 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 α-메틸 스티렌을 유량 30 kg/hr로 스프레이 하였다.After separating the volatile components under the separation condition A, the separated volatile components were condensed to the first condenser under the condensation condition A, and then the uncondensed volatile components were transferred to the second condenser and condensed. At this time, the volatile component separated from the volatilization tank is not sprayed on the volatile component being transferred to the first condenser, and α-methyl styrene is flowed to the volatile component that is not condensed on the first condenser and is being transferred to the second condenser at a flow rate of 30 kg/hr. Was sprayed with.
**
실시예 4Example 4
분리조건 A 하에서 휘발성 성분을 분리한 다음, 분리된 휘발성 성분을 응축조건 A 하에서 제1 응축기로 응축 후 응축되지 않은 휘발성 성분을 제2 응축기로 이송하여 응축하였다. 이 때, 휘발조에서 분리된 휘발성 성분을 제1 응축기로 이송 중인 휘발성 성분에는 스프레이 하지 않고, 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 톨루엔을 유량 80 kg/hr로 스프레이 하였다.After separating the volatile components under the separation condition A, the separated volatile components were condensed to the first condenser under the condensation condition A, and then the uncondensed volatile components were transferred to the second condenser and condensed. At this time, the volatile components separated from the volatile tank were not sprayed on the volatile components being transferred to the first condenser, and toluene was sprayed on the volatile components not being condensed on the first condenser and being transferred to the second condenser at a flow rate of 80 kg/hr. .
*실시예 5 * Example 5
분리조건 A 하에서 휘발성 성분을 분리한 후, 분리된 휘발성 성분을 응축조건 A 하에서 제1 응축기로 응축 후 응축되지 않은 휘발성 성분을 제2 응축기로 이송하여 응축하였다. 이 때, 휘발조에서 분리되어 제1 응축기로 이송 중인 휘발성 성분에 톨루엔을 유량 20 kg/hr로 스프레이하고, 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 스티렌을 유량 15 kg/hr로 스프레이 하였다.After separating the volatile components under the separation condition A, the separated volatile components were condensed to the first condenser under the condensing condition A, and then the uncondensed volatile components were transferred to the second condenser to condense. At this time, toluene is sprayed at a flow rate of 20 kg/hr to the volatile components separated from the volatilization tank and transported to the first condenser. Sprayed with hr.
*실시예 6 내지 21 * Examples 6 to 21
하기 표 1 내지 3에 기재된 바와 같은 분리조건 및 응축조건으로 휘발성 성분을 분리 및 응축하고 휘발성 성분에 스프레이 물질을 스프레이 하였다.The volatile components were separated and condensed under separation conditions and condensation conditions as described in Tables 1 to 3 below, and spray materials were sprayed on the volatile components.
비교예 1Comparative Example 1
실시예 1에서 휘발조에서 분리되어 제1 응축기로 이송 중인 휘발성 성분에 톨루엔을 스프레이 하지 않은 것을 제외하고는 상기 실시예 1과 동일하게 수행하였다.It was performed in the same manner as in Example 1, except that toluene was not sprayed on the volatile component separated from the volatile tank in Example 1 and being transferred to the first condenser.
비교예 2 내지 16Comparative Examples 2 to 16
하기 표 4 내지 5에 기재된 바와 같은 분리조건 및 응축조건으로 휘발성 성분을 분리 및 응축하고 휘발성 성분에 스프레이 물질을 스프레이 하였다.The volatile components were separated and condensed under separation conditions and condensation conditions as described in Tables 4 to 5 below, and spray materials were sprayed on the volatile components.
[시험예][Test Example]
상기 실시예 1 내지 21 및 비교예 1 내지 16에서 제2 응축기로부터 응축되지 않고 배출된 휘발성 성분의 유량을 제2 응축기와 진공 유닛 사이에 설치된 유량계로 측정하여 하기 표 1 내지 5에 나타내었다.In Examples 1 to 21 and Comparative Examples 1 to 16, the flow rate of volatile components discharged without being condensed from the second condenser was measured with a flow meter installed between the second condenser and the vacuum unit, and the results are shown in Tables 1 to 5 below.
또한, 상기 실시예 1 내지 14 및 비교예 1 내지 16에서 제1 응축기에서 응축되지 않고 제2 응축기로 이송된 비닐시안 단량체의 함량은 제1 응축기에서 제2 응축기로 이송되는 배관에서 샘플링하여, 가스 크로마토그래피로 정량분석하여 하기 표 1 내지 5에 나타내었다.In addition, in Examples 1 to 14 and Comparative Examples 1 to 16, the content of the vinyl cyan monomer not condensed in the first condenser and transferred to the second condenser is sampled in a pipe transferred from the first condenser to the second condenser, and then gas Quantitative analysis by chromatography is shown in Tables 1 to 5 below.
구분division 실시예Example
1One 22 33 44 55 66 77
휘발조의 분리조건Separation conditions of gasoline AA AA AA AA AA AA AA
응축기의 응축조건Condensing condition of condenser AA AA AA AA AA AA AA
제1 응축기로 이송 중인 휘발성 성분에 스프레이 하는 물질Substance sprayed on volatile components being transported to the first condenser 1One -- -- -- 1One 1One 1One
제1 응축기로 이송 중인 휘발성 성분에스프레이 하는 물질의 유량(kg/hr)Flow rate of material sprayed on volatile components being transported to the first condenser (kg/hr) 4545 -- -- -- 2020 2020 3030
제2 응축기로 이송 중인 휘발성 성분에스프레이 하는 물질Materials spraying volatile components being transported to the second condenser -- 22 33 1One 22 33 1One
제2 응축기로 이송 중인 휘발성 성분에스프레이 하는 물질의 유량(kg/hr)Flow rate of material sprayed on volatile components being transported to the second condenser (kg/hr) -- 3030 3030 8080 1515 1515 3030
제1 응축기에서 응축되지 않고 제2 응축기로 이송된 비닐시안 단량체의 함량(중량%)Content of vinyl cyanide monomer (weight %) transferred to the second condenser without being condensed in the first condenser 12.512.5 13.013.0 13.013.0 11.811.8 12.912.9 12.912.9 12.212.2
제2 응축기에서 응축되지 않고 배출되는 휘발성 성분의 유량(kg/hr)Flow rate of volatile components discharged without condensation from the second condenser (kg/hr) 00 00 00 00 00 00 00
구분division 실시예Example
88 99 1010 1111 1212 1313 1414
휘발조의 분리조건Separation conditions of gasoline BB BB BB BB BB BB BB
응축기의 응축조건Condensing condition of condenser BB BB BB BB BB BB BB
제1 응축기로 이송 중인 휘발성 성분에스프레이 하는 물질Material spraying volatile components being transported to the first condenser 1One -- -- -- 1One 1One 1One
제1 응축기로 이송중인 휘발성 성분에스프레이 하는 물질의유량(kg/hr)Flow rate of material sprayed on volatile components being transported to the first condenser (kg/hr) 3030 -- -- -- 1010 1010 1010
제2 응축기로 이송 중인 휘발성 성분에스프레이 하는 물질Materials spraying volatile components being transported to the second condenser -- 22 33 1One 22 33 1One
제2 응축기로 이송 중인 휘발성 성분에 스프레이 하는 물질의 유량(kg/hr)Flow rate of material sprayed on volatile components being transported to the second condenser (kg/hr) -- 1010 1212 1414 1010 1010 1010
제1 응축기에서 응축되지 않고 제2 응축기로 이송된 비닐시안 단량체의 함량(중량%)Content of vinyl cyanide monomer not condensed in the first condenser and transferred to the second condenser (% by weight) 52.952.9 53.453.4 53.153.1 52.752.7 52.752.7 52.752.7 52.752.7
제2 응축기에서 응축되지 않고 배출되는 휘발성 성분의 유량 (kg/hr)Flow rate of volatile components discharged without condensation from the second condenser (kg/hr) 00 00 00 00 00 00 00
구분division 실시예Example
1515 1616 1717 1818 1919 2020 2121
휘발조의 분리조건Separation conditions of gasoline CC CC CC CC CC CC CC
응축기의 응축조건Condensing condition of condenser CC CC CC CC CC CC CC
제1 응축기로 이송 중인 휘발성 성분에 스프레이 하는 물질Substance sprayed on volatile components being transported to the first condenser 1One -- -- -- 1One 1One 1One
제1 응축기로 이송 중인 휘발성 성분에 스프레이 하는 물질의 유량(kg/hr)Flow rate of material sprayed on volatile components being transported to the first condenser (kg/hr) 150150 -- -- -- 6565 6565 9090
제2 응축기로 이송중인 휘발성 성분에스프레이 하는 물질Material spraying volatile components being transported to the second condenser -- 22 33 1One 22 33 1One
제2 응축기로 이송 중인 휘발성 성분에스프레이 하는 물질의 유량(kg/hr)Flow rate of material sprayed on volatile components being transported to the second condenser (kg/hr) -- 110110 110110 215215 6565 6565 9090
제1 응축기에서 응축되지 않고 제2 응축기로 이송된 비닐시안 단량체의 함량(중량%)Content of vinyl cyanide monomer not condensed in the first condenser and transferred to the second condenser (% by weight) 19.719.7 21.521.5 21.521.5 18.418.4 20.720.7 20.720.7 19.219.2
제2 응축기에서 응축되지 않고 배출되는 휘발성 성분의 유량 (kg/hr)Flow rate of volatile components discharged without condensation from the second condenser (kg/hr) 00 00 00 00 00 00 00
구분division 비교예Comparative example
1One 22 33 44 55 66 77 88
휘발조의 분리조건Separation conditions of gasoline AA AA AA AA AA AA AA BB
응축기의 응축조건Condensing condition of condenser AA AA AA AA AA AA AA BB
제1 응축기로 이송 중인 휘발성 성분에스프레이 하는 물질Material spraying volatile components being transported to the first condenser -- 22 33 44 55 -- -- --
제1 응축기로 이송 중인 휘발성 성분에스프레이 하는 물질의 유량(kg/hr)Flow rate of material sprayed on volatile components being transported to the first condenser (kg/hr) -- 3030 3030 3030 3030 -- -- --
제2 응축기로 이송 중인 휘발성 성분에 스프레이 하는 물질Substance sprayed on volatile components being transported to the second condenser -- -- -- -- -- 44 55 --
제2 응축기로 이송 중인 휘발성 성분에스프레이 하는 물질의 유량(kg/hr)Flow rate of material sprayed on volatile components being transported to the second condenser (kg/hr) -- -- -- -- -- 3030 3030 --
제1 응축기에서 응축되지 않고 제2 응축기로 이송된 비닐시안 단량체의 함량(중량%)Content of vinyl cyanide monomer not condensed in the first condenser and transferred to the second condenser (% by weight) 13.913.9 14.214.2 14.514.5 16.616.6 17.017.0 19.519.5 19.519.5 55.355.3
제2 응축기에서 응축되지 않고 배출되는 휘발성 성분의 유량 (kg/hr)Flow rate of volatile components discharged without condensation from the second condenser (kg/hr) 15.015.0 17.117.1 22.322.3 52.052.0 17.017.0 86.886.8 41.641.6 14.814.8
구분division 비교예Comparative example
99 1010 1111 1212 1313 1414 1515 1616
휘발조의 분리조건Separation conditions of gasoline BB BB BB CC CC CC CC CC
응축기의 응축조건Condensing condition of condenser BB BB BB CC CC CC CC CC
제1 응축기로 이송 중인 휘발성 성분에 스프레이 하는 물질Substance sprayed on volatile components being transported to the first condenser 22 44 -- -- 22 33 44 --
제1 응축기로 이송 중인 휘발성 성분에 스프레이 하는물질의 유량(kg/hr)Flow rate of material sprayed on volatile components being transported to the first condenser (kg/hr) 3030 3030 -- -- 150150 150150 150150 --
제2 응축기로 이송 중인 휘발성 성분에 스프레이 하는 물질Substance sprayed on volatile components being transported to the second condenser -- -- 44 -- -- -- -- 55
제2 응축기로 이송 중인 휘발성 성분에 스프레이 하는물질의 유량(kg/hr)Flow rate of material sprayed on volatile components being transported to the second condenser (kg/hr) -- -- 3030 -- -- -- -- 110110
제1 응축기에서 응축되지 않고 제2 응축기로 이송된 비닐시안 단량체의 함량(중량%)Content of vinyl cyanide monomer not condensed in the first condenser and transferred to the second condenser (% by weight) 55.555.5 55.855.8 59.759.7 26.226.2 27.227.2 29.729.7 31.931.9 39.339.3
제2 응축기에서 응축되지 않고 배출되는 휘발성 성분의 유량 (kg/hr)Flow rate of volatile components discharged without condensation from the second condenser (kg/hr) 15.415.4 21.021.0 51.351.3 58.058.0 59.959.9 80.580.5 177.8177.8 129.7129.7
상기 표 1 내지 5에 나타낸 바와 같이, 본 기재에 따른 실시예 1 내지 21은 제2 응축기로부터 응축되지 않고 배출되는 휘발성 성분이 없으므로 이를 처리하기 위해 폐수 처리 비용이 필요치 않음을 확인할 수 있었다.반면에, 종래의 방법에 의한 비교예 1, 8 및 12은 제2 응축기로부터 응축되지 않은 휘발성 성분이 14.8 내지 58.0 kg/hr로 많은 양이 배출되었다.As shown in Tables 1 to 5, Examples 1 to 21 according to the present disclosure could be confirmed that there is no volatile component discharged without being condensed from the second condenser, so it is confirmed that the wastewater treatment cost is not required to treat it. , In Comparative Examples 1, 8 and 12 according to the conventional method, a large amount of volatile components not condensed from the second condenser was discharged at 14.8 to 58.0 kg/hr.
또한, 제1 응축기에 방향족 비닐 단량체를 스프레이한 경우(비교예 2, 3, 9, 13 및 14) 및 제1 응축기에 비닐시안 단량체를 스프레이한 경우(비교예 4, 5, 10 및 15)는, 제2 응축기로부터 응축되지 않고 배출되는 휘발성 성분의 함량이 급격히 증가하여 이를 처리하기 위한 비용이 많이 소모됨을 확인할 수 있었다.In addition, when the aromatic vinyl monomer was sprayed to the first condenser (Comparative Examples 2, 3, 9, 13 and 14) and when the vinyl cyan monomer was sprayed to the first condenser (Comparative Examples 4, 5, 10 and 15), , It has been confirmed that the content of volatile components discharged without being condensed from the second condenser is rapidly increased, and thus, a cost for processing the same is consumed.
또한, 제2 응축기에 비닐시안 단량체를 스프레이한 비교예 6, 7, 11 및 16도 마찬가지로 제2 응축기로부터 응축되지 않고 배출되는 휘발성 성분의 함량이 크게 증가하였다.In addition, in Comparative Examples 6, 7, 11, and 16 in which the vinyl cyan monomer was sprayed on the second condenser, the content of volatile components discharged without being condensed from the second condenser was also greatly increased.

Claims (13)

  1. 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체, 잔류 비닐시안 단량체 및 유기 용매를 포함하는 중합 생성물을 휘발조를 이용하여 휘발성 성분을 분리하는 단계; 및Separating a volatile component using a volatilization tank for a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent; And
    분리된 휘발성 성분을 1개 또는 직렬로 연결된 2개 이상의 응축기를 이용하여 응축하는 단계;를 포함하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법으로서, A method for producing an aromatic vinyl compound-vinyl cyan compound polymer comprising: condensing separated volatile components using one or two or more condensers connected in series.
    상기 휘발조에서 분리되어 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계; 또는 Spraying an organic solvent to a volatile component separated from the volatile tank and being transported to a condenser; or
    상기 직렬로 연결된 2개 이상의 응축기를 이용할 때 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계;를 포함하는 것을 특징으로 하는When using two or more condensers connected in series, spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser.
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법.Method for producing aromatic vinyl compound-vinyl cyan compound polymer.
  2. 제1항에 있어서,According to claim 1,
    상기 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법은, 상기 휘발조에서 분리되어 제1 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계; 및 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계;를 포함하는 것을 특징으로 하는 The method for preparing the aromatic vinyl compound-vinyl cyan compound polymer includes spraying an organic solvent to a volatile component separated from the volatile tank and being transferred to a first condenser; And spraying an organic solvent or an aromatic vinyl monomer to a volatile component that is not condensed in the first condenser and is being transferred to the second condenser.
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법.Method for producing aromatic vinyl compound-vinyl cyan compound polymer.
  3. 제1항에 있어서,According to claim 1,
    상기 분리된 휘발성 성분은 비닐시안 화합물 5 내지 35 중량%, 방향족 비닐 화합물 45 내지 80 중량% 및 유기 용매 5 내지 50 중량% 포함하는 것을 특징으로 하는 The separated volatile component is characterized in that it comprises 5 to 35% by weight of vinyl cyan compound, 45 to 80% by weight of aromatic vinyl compound and 5 to 50% by weight of organic solvent
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법.Method for producing aromatic vinyl compound-vinyl cyan compound polymer.
  4. 제1항에 있어서, According to claim 1,
    상기 휘발조에서 분리되어 제1 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계는, 유기 용매를 유량 10 내지 200 Kg/hr로 스프레이 하는 것을 특징으로 하는 The step of spraying the organic solvent to the volatile components separated from the volatilization tank and being transported to the first condenser is characterized in that the organic solvent is sprayed at a flow rate of 10 to 200 Kg/hr.
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법.Method for producing aromatic vinyl compound-vinyl cyan compound polymer.
  5. 제1항에 있어서,According to claim 1,
    상기 휘발조에서 분리되어 제1 응축기로 이송 중인 휘발성 성분에 유기 용매를 스프레이 하는 단계는, 유기 용매를 온도 -10℃ 내지 40℃로 스프레이 하는 것을 특징으로 하는 The step of spraying the organic solvent to the volatile components separated from the volatilization tank and being transported to the first condenser is characterized in that the organic solvent is sprayed at a temperature of -10°C to 40°C.
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법.Method for producing aromatic vinyl compound-vinyl cyan compound polymer.
  6. 제1항에 있어서, According to claim 1,
    상기 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계는, 유기용매 또는 방향족 비닐 단량체를 유량 10 내지 220 Kg/hr 범위 내로 스프레이 하는 것을 특징으로 하는 The step of spraying the organic solvent or the aromatic vinyl monomer to the volatile components that are not condensed in the first condenser and being transferred to the second condenser is characterized in that the organic solvent or the aromatic vinyl monomer is sprayed within a flow rate of 10 to 220 Kg/hr. doing
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법.Method for producing aromatic vinyl compound-vinyl cyan compound polymer.
  7. 제1항에 있어서, According to claim 1,
    상기 제1 응축기에서 응축되지 않고 제2 응축기로 이송 중인 휘발성 성분에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 단계는, 유기용매 또는 방향족 비닐 단량체를 온도 -10℃ 내지 40℃로 스프레이 하는 것을 특징으로 하는 The step of spraying the organic solvent or the aromatic vinyl monomer to the volatile component that is not condensed in the first condenser and being transferred to the second condenser is characterized in that the organic solvent or the aromatic vinyl monomer is sprayed at a temperature of -10°C to 40°C.
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법.Method for producing aromatic vinyl compound-vinyl cyan compound polymer.
  8. 제1항에 있어서,According to claim 1,
    상기 제1 응축기에서 응축은 냉매 온도 20℃ 내지 35℃ 및 운전압력 3 내지 100 torr 하에서 수행되는 것을 특징으로 하는 Condensation in the first condenser is characterized in that is carried out under the refrigerant temperature 20 ℃ to 35 ℃ and operating pressure 3 to 100 torr
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법.Method for producing aromatic vinyl compound-vinyl cyan compound polymer.
  9. 제1항에 있어서, According to claim 1,
    상기 제2 응축기에서 응축은 냉매 온도 -3℃ 내지 4℃ 및 운전압력 5 내지 50 torr 하에서 수행되는 것을 특징으로 하는 Condensation in the second condenser is characterized in that is performed under the refrigerant temperature -3 ℃ to 4 ℃ and operating pressure 5 to 50 torr
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법.Method for producing aromatic vinyl compound-vinyl cyan compound polymer.
  10. 제1항에 있어서,According to claim 1,
    상기 휘발조에서 휘발성 성분을 분리하는 단계는 온도 220 내지 260℃ 및 압력 35 torr 이하의 조건 하에서 수행되는 것을 특징으로 하는 The step of separating the volatile components from the volatile bath is characterized in that it is performed under conditions of a temperature of 220 to 260°C and a pressure of 35 torr or less.
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법.Method for producing aromatic vinyl compound-vinyl cyan compound polymer.
  11. 제1항에 있어서, According to claim 1,
    상기 제1 응축기 및 제2 응축기에서 응축된 응축물은 회수 및 정제되어 반응기로 재투입 되는 것을 특징으로 하는 The condensate condensed in the first condenser and the second condenser is recovered and purified and re-entered into the reactor.
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조방법.Method for producing aromatic vinyl compound-vinyl cyan compound polymer.
  12. 방향족 비닐 화합물-비닐시안 화합물 중합체, 잔류 방향족 비닐 단량체, 잔류 비닐시안 단량체 및 유기 용매를 포함하는 중합 생성물로부터 휘발성 성분을 분리하는 휘발조; 및A volatilization tank for separating volatile components from a polymerization product comprising an aromatic vinyl compound-vinyl cyan compound polymer, a residual aromatic vinyl monomer, a residual vinyl cyan monomer, and an organic solvent; And
    상기 분리된 휘발성 성분을 응축시키는 1개 또는 직렬로 연결된 2개 이상의 응축기;를 포함하는 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조장치로,An apparatus for producing an aromatic vinyl compound-vinyl cyan compound polymer comprising: one or two or more condensers connected in series to condense the separated volatile components,
    상기 분리된 휘발성 성분을 응축기로 이송하는 이송배관에 유기 용매를 스프레이 하는 스프레이 수단을 포함하거나, It includes a spray means for spraying the organic solvent to the transport pipe for transporting the separated volatile components to the condenser,
    상기 직렬로 연결된 2개 이상의 응축기를 포함할 때 제1 응축기에서 응축되지 않은 휘발성 성분을 제2 응축기로 이송하는 이송배관에 유기 용매 또는 방향족 비닐 단량체를 스프레이 하는 스프레이 수단을 포함하는 것을 특징으로 하는When including two or more condensers connected in series, characterized in that it comprises a spray means for spraying an organic solvent or an aromatic vinyl monomer to the transport pipe for transporting the volatile components that are not condensed in the first condenser to the second condenser.
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조장치.Apparatus for producing aromatic vinyl compound-vinyl cyan compound polymer.
  13. 제12항에 있어서,The method of claim 12,
    상기 방향족 비닐 화합물-비닐시안 화합물 중합체의 제조장치는 상기 분리된 휘발성 성분을 제1 응축기로 이송하는 이송배관에 유기용매를 스프레이 하는 스프레이 배관을 포함하고, 제1 응축기에서 응축되지 않은 휘발성 성분을 제2 응축기로 이송하는 이송배관에 유기용매 또는 방향족 비닐 단량체를 스프레이 하는 스프레이 배관을 포함하는 것을 특징으로 하는The apparatus for producing the aromatic vinyl compound-vinyl cyan compound polymer includes a spray pipe for spraying an organic solvent to a transport pipe for transporting the separated volatile component to the first condenser, and removes volatile components not condensed in the first condenser. 2 It characterized in that it comprises a spray pipe for spraying an organic solvent or an aromatic vinyl monomer to the transfer pipe to the condenser
    방향족 비닐 화합물-비닐시안 화합물 중합체의 제조장치.Apparatus for producing aromatic vinyl compound-vinyl cyan compound polymer.
PCT/KR2019/009587 2018-12-18 2019-08-01 Manufacturing method and device for aromatic vinyl compound-vinyl cyanide compound polymer WO2020130264A1 (en)

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