JPH0148283B2 - - Google Patents
Info
- Publication number
- JPH0148283B2 JPH0148283B2 JP56015969A JP1596981A JPH0148283B2 JP H0148283 B2 JPH0148283 B2 JP H0148283B2 JP 56015969 A JP56015969 A JP 56015969A JP 1596981 A JP1596981 A JP 1596981A JP H0148283 B2 JPH0148283 B2 JP H0148283B2
- Authority
- JP
- Japan
- Prior art keywords
- polymerization vessel
- water
- gas
- monomer
- vessel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
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- 238000006116 polymerization reaction Methods 0.000 claims description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000000178 monomer Substances 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 13
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical group ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 7
- -1 vinyl compound Chemical class 0.000 claims description 6
- 229920002554 vinyl polymer Polymers 0.000 claims description 6
- 239000012736 aqueous medium Substances 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000002075 main ingredient Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 230000000379 polymerizing effect Effects 0.000 claims 1
- 239000007789 gas Substances 0.000 description 16
- 238000010408 sweeping Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000010276 construction Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical group CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Description
【発明の詳細な説明】
本発明はビニル化合物を重合器中において水性
媒体中で重合して得られた重合体スラリーを前記
重合器から抜出した後の該重合器内に残留するビ
ニル化合物モノマー（以后単にモノマーと記す）
の重合器からの排除及び回収方法に関するもので
ある。DETAILED DESCRIPTION OF THE INVENTION The present invention deals with the treatment of vinyl compound monomers ( (hereinafter simply referred to as monomer)
The present invention relates to a method for removing and recovering from a polymerization vessel.
従来、ビニル化合物を重合器中において水性媒
体中で重合した後、未反応モノマーを重合器上部
より回収し、或いは回収することなしに、前記重
合によつて得られたスラリーを下部より抜出して
いる。その後次バツチのスタートまでに器壁等に
付着したスケールを除くためにマンホールを開放
して高圧水により洗浄する或いは人間が重合器内
に入つて作業することがある。しかしながら、ス
ラリー抜出後の重合器内に残留するモノマーの量
は一般に高濃度であり、労動衛生上作業環境濃度
としては極めて不適当である。そこで、この重合
器内に残留するモノマーを除去し、又は回収する
方法として、以下に示すようないくつかの方法が
行なわれ又は提案されている。 Conventionally, after a vinyl compound is polymerized in an aqueous medium in a polymerization vessel, unreacted monomers are collected from the top of the polymerization vessel, or the slurry obtained by the polymerization is extracted from the bottom without recovering them. . Thereafter, in order to remove scale adhering to the vessel walls and the like before the start of the next batch, the manhole may be opened and washed with high-pressure water, or a person may enter the polymerization vessel to work. However, the amount of monomer remaining in the polymerization vessel after the slurry is discharged is generally high in concentration, which is extremely inappropriate as a concentration in the working environment in terms of occupational hygiene. Therefore, as a method for removing or recovering the monomer remaining in the polymerization vessel, several methods as shown below have been carried out or proposed.
吸引ブロワーにより重合器内ガスを吸引排気
即ち空気置換する。 The gas inside the polymerization reactor is suctioned out, or replaced with air, by a suction blower.
重合器内に窒素ガスを導入し、重合器内ガス
を追出す。排気中のモノマーは活性炭吸着によ
り回収する。この方法は例えば、特開昭53―
36587に記載されている。 Introduce nitrogen gas into the polymerization vessel and expel the gas inside the polymerization vessel. Monomers in the exhaust gas are recovered by activated carbon adsorption. This method, for example,
Listed in 36587.
重合器内に水を導入し、器内残留塩化ビニル
モノマーを追出す。この方法は例えば、特開昭
53―36585に記載されている。 Water is introduced into the polymerization vessel and residual vinyl chloride monomer inside the vessel is expelled. This method is used, for example, in
53-36585.
重合器上部よりスチームを吹込み、下部より
排気する。この方法は例えば、特開昭52―
36605及び特開昭53―36586に記載されている。 Steam is blown into the polymerization vessel from the top and exhausted from the bottom. This method, for example,
36605 and JP-A No. 53-36586.
これらの方法はそれぞれ問題点を有する。即
ち、はモノマーの量によつては、爆鳴気を生成
する恐れがあり、また排気中のモノマーを回収す
ることは、一般に困難である。 Each of these methods has its own problems. That is, depending on the amount of monomer, there is a risk of generating explosive gas, and it is generally difficult to recover the monomer in the exhaust gas.
は排気中のモノマーを回収する活性炭吸着装
置が相当額の建設費を要し、かつ活性炭の再生に
伴なうランニングコストも無視できない。 Activated carbon adsorption equipment that recovers monomers from exhaust gas requires considerable construction costs, and the running costs associated with regenerating activated carbon cannot be ignored.
は、水を導入するポンプ及びその水を保有す
る貯槽等を必要とし、装置が大がかりとなり、ま
たポンプの動力費も無視できない。更に、水に溶
け込んだモノマーを除去するため、この水をスト
リツパーで処理せねばならず、装置・熱の費用が
かさむ。 This requires a pump to introduce water and a storage tank to hold the water, making the equipment large-scale and the cost of powering the pump cannot be ignored. Furthermore, in order to remove monomers dissolved in the water, this water must be treated with a stripper, increasing equipment and heat costs.
は、，に比べれば、建設費が比較的小さ
いが、スチームを系内に導入する配管及び重合器
下部より排気を導出する配管を必要とし、それだ
け建設費が増加する。 The construction cost is relatively small compared to , but it requires piping to introduce steam into the system and piping to take out the exhaust gas from the lower part of the polymerization reactor, which increases the construction cost accordingly.
本発明の目的は重合器中に残留するモノマーを
短時間に重合器から排除（スイーピング）し、か
つ、回収する方法であつて、高度に経済的な方法
を提供することである。 An object of the present invention is to provide a highly economical method for sweeping and recovering monomers remaining in a polymerization vessel in a short period of time.
本発明はビニル化合物の重合体のスラリーを重
合器から抜出し、その後重合器内に水を注入し、
所望により加熱しながら、重合器上部より重合器
内のガスを吸引することにより、残留するモノマ
ーを水蒸気により排除（スイーピング）し、前記
重合器内ガスの吸引排出の間、重合器内のガスを
撹拌するため、重合器内撹拌器を回転させ、前記
排出したガスを段階的に凝縮させるものである。 The present invention involves extracting a slurry of a vinyl compound polymer from a polymerization vessel, then injecting water into the polymerization vessel,
By suctioning the gas inside the polymerization vessel from the upper part of the polymerization vessel while heating if desired, the remaining monomer is removed by steam (sweeping). For stirring, a stirrer in the polymerization vessel is rotated, and the discharged gas is condensed in stages.
本発明に適用しうるモノマーは水性媒体中で重
合しうるものなら、何でもよく、例として、塩化
ビニル、スチレン、酢酸ビニル、等
を挙げることができる。 The monomer applicable to the present invention may be any monomer as long as it can be polymerized in an aqueous medium, and examples thereof include vinyl chloride, styrene, vinyl acetate, and the like.
重合器内に注入する水は、仕込水用配管、スラ
リー洗浄用配管あるいは重合撹拌機メカニカルシ
ール用注水配管等既設の配管を経由して重合器内
に注入することができる。水の注入は当初に全量
を行なつてもよく、スイーピングの間連続的に行
なつてもよい。連続的に注入する場合の水量は重
合器単位容積（m3）当り、0.1〜50／hr好まし
くは１〜10／hrが適当である。水量が小さ過ぎ
るとモノマーの排除が不充分である。一方大き過
ぎるのは不経済である。重合器に注入した水の加
熱は重合器のジヤケツトに温水を通じることによ
り行ない、もしくは、あらかじめ加熱した水を注
水することのいずれか、又は、両者の併用が行な
われる。加熱を重合器のジヤケツトに温水を通じ
ることにより行なうときは注入水が所望の温度に
上がる迄、重合器内に設備された撹拌器で注入水
を撹拌するのが好ましい。 Water to be injected into the polymerization vessel can be injected into the polymerization vessel via existing piping such as a feed water piping, a slurry cleaning piping, or a water injection piping for a polymerization agitator mechanical seal. Injection of water can be done in its entirety initially or continuously during sweeping. When injecting water continuously, the appropriate amount of water is 0.1 to 50/hr, preferably 1 to 10/hr, per unit volume (m 3 ) of the polymerization reactor. If the amount of water is too small, monomer removal will be insufficient. On the other hand, being too large is uneconomical. The water injected into the polymerization vessel is heated either by passing hot water through the jacket of the polymerization vessel, by injecting preheated water, or by a combination of both. When heating is carried out by passing hot water through the jacket of the polymerization vessel, it is preferable to stir the injected water with a stirrer installed in the polymerization vessel until the injected water reaches the desired temperature.
重合器内に注入した水の温度は30〜90℃の温度
範囲が適当である。30℃以下では水の蒸発量が不
十分であり、90℃以上では器内壁に附着している
重合体のスケールが固着する恐れがあるから適当
でない。 The temperature of the water injected into the polymerization vessel is suitably in the range of 30 to 90°C. If the temperature is below 30°C, the amount of water evaporated will be insufficient, and if it is above 90°C, the polymer scale adhering to the inner wall of the vessel may stick, so it is not suitable.
重合器内のガスの吸引量は、重合器の単位容積
（m3）当り0.1〜50Nm3／hr好ましくは１〜10N
m3／hrがよい。0.1Nm3／hrより小さいときはモ
ノマーの排除が不充分であり、一方50Nm3／hrよ
り大きいときは過度に大きなブロワーを要しまた
モノマー排除の効率が悪くなるので好ましくな
い。 The amount of gas sucked into the polymerization vessel is 0.1 to 50Nm 3 /hr, preferably 1 to 10N per unit volume (m 3 ) of the polymerization vessel.
m 3 /hr is good. When it is less than 0.1 Nm 3 /hr, monomer removal is insufficient, while when it is more than 50 Nm 3 /hr, an excessively large blower is required and the efficiency of monomer removal becomes poor, which is not preferable.
重合器内圧力は通常0.05〜２Kg／cm2―abs.程度
である。重合器内ガスの吸引の当初は器内残留モ
ノマー猫度が高いから、器内圧力も高いがガス吸
引の終りの頃は器内圧力は低くなり器内に注入さ
れた水の飽和水蒸気圧に近い値になる。ガス吸引
の終りの頃において器内圧力を0.05Kg／cm2―abs.
より小にするには高真空の排気ブロワーを必要と
し、建設費が大となるから好ましくない。 The pressure inside the polymerization vessel is usually about 0.05 to 2 Kg/cm 2 -abs. At the beginning of the suction of gas in the polymerization vessel, the residual monomer concentration in the vessel is high, so the pressure inside the vessel is high, but at the end of gas suction, the pressure inside the vessel decreases and the saturated water vapor pressure of the water injected into the vessel is reached. The values will be close. At the end of gas suction, the pressure inside the chamber was reduced to 0.05Kg/cm 2 - abs.
Making it even smaller requires a high-vacuum exhaust blower, which is undesirable because it increases construction costs.
蒸発した水は重合器内に残留するモノマーを同
伴しながら重合器上部から排出されることにな
る。この排出の間、重合器内にデツドスペースを
作らないようにするため、又水蒸気より重いモノ
マーを効率的に重合器上部より排出するため、重
合器内の撹拌器を回す。 The evaporated water is discharged from the upper part of the polymerization vessel, taking with it the monomer remaining in the polymerization vessel. During this discharge, the stirrer inside the polymerization vessel is turned so as not to create a dead space within the polymerization vessel and to efficiently discharge monomers heavier than water vapor from the top of the polymerization vessel.
重合器上部より器内ガスを吸引するラインに
は、排気ブロワーが設けられ、このブロワーによ
り、重合器内ガスを吸引する。吸引は好ましくは
負圧吸引により行なう。前記排気ブロワーのサク
シヨン側にコンデンサーを設置し、水蒸気を凝縮
させ、モノマーを回収するのがよい。ただしこの
排気ブロワーとしてナツシユポンプ（液封型真空
ポンプ）を使う場合には、必らずしもブロワーの
前に水コンデンサーを設置する必要はない。前記
器内ガス吸引ラインは重合終了時に未反応モノマ
ーを回収するラインを代用することができる。こ
の未反応モノマー回収ラインは、通常負圧回収用
のナツシユポンプを備えている。 An exhaust blower is provided in the line for sucking the gas inside the polymerization vessel from the upper part of the polymerization vessel, and this blower sucks the gas inside the polymerization vessel. Suction is preferably performed by negative pressure suction. It is preferable to install a condenser on the suction side of the exhaust blower to condense water vapor and recover the monomer. However, when using a Natsushi pump (liquid ring vacuum pump) as the exhaust blower, it is not necessarily necessary to install a water condenser in front of the blower. The in-vessel gas suction line can be replaced by a line for recovering unreacted monomers at the end of polymerization. This unreacted monomer recovery line is usually equipped with a nutsch pump for negative pressure recovery.
水蒸気と共に吸引されたモノマーは排気ブロワ
ーを経て、回収装置へ送られ、回収され再使用さ
れる。このスイーピングに要する時間は、スラリ
ー抜出後の重合器内モノマー量及びスイーピング
後の許容モノマー残留量によつて異なるが、通常
５〜60分の範囲の時間が適当である。 The monomer sucked together with water vapor is sent to a recovery device via an exhaust blower, where it is recovered and reused. The time required for this sweeping varies depending on the amount of monomer in the polymerization vessel after the slurry is discharged and the allowable amount of monomer remaining after sweeping, but is usually in the range of 5 to 60 minutes.
以上述べてきた通り、本発明の特徴は重合器内
に残留する未反応モノマーを回収するに当り、特
別の装置、配管を必要とすることなしに、即ち、
高度に経済的に、かつ効率良く重合器内をスイー
ピング処理できる所にある。 As described above, the feature of the present invention is that unreacted monomers remaining in the polymerization vessel can be recovered without requiring any special equipment or piping.
It is located in a place where the inside of the polymerization vessel can be swept in a highly economical and efficient manner.
実施例 １
25m3のステンレス製重合器に、水、ポリビニル
アルコール、２―エチルヘキシルパーオキシジカ
ルボネート、塩化ビニルモノマーを仕込み、58℃
まで昇温し、重合反応を行なつた。８時間後重合
反応終了し、未反応塩化ビニルモノマーを内温58
℃に保つた状態で内圧が、1.0Kg／cm2―abs.にな
るまで回収した。引続き負圧回収しながらスラリ
ーを抜出した。この時の系内の状態は温度：50
℃、圧力；0.30Kg／cm2―abs.，塩化ビニルモノマ
ーの分圧：0.18Kg／cm2―abs.であつた。Example 1 Water, polyvinyl alcohol, 2-ethylhexyl peroxydicarbonate, and vinyl chloride monomer were charged into a 25 m 3 stainless steel polymerization vessel, and heated to 58°C.
The polymerization reaction was carried out. After 8 hours, the polymerization reaction was completed and the unreacted vinyl chloride monomer was cooled to an internal temperature of 58.
The sample was collected while being kept at ℃ until the internal pressure reached 1.0Kg/cm 2 -abs. The slurry was then extracted while recovering negative pressure. The state inside the system at this time is temperature: 50
°C, pressure: 0.30Kg/cm 2 -abs., partial pressure of vinyl chloride monomer: 0.18Kg/cm 2 -abs.
これより器内へ温度20℃の水を200／hrの流
量で注入し、重合器のジヤケツトに90℃の温水を
循環させ、重合器上部から引続きナツシユポンプ
により、負圧吸引（約7Nm3／hr）を行ないなが
ら器内スイーピングを行なつた。30分経過後スイ
ーピングを終了した。この時の状態は器内温度：
60℃、器内圧力：0.30Kg／cm2―abs.，塩化ビニル
モノマー分圧：0.0001Kg／cm2―abs.となつた。 From this point, water at a temperature of 20°C is injected into the vessel at a flow rate of 200°C/hr, and hot water at 90°C is circulated through the jacket of the polymerization vessel, followed by negative pressure suction (approximately 7Nm 3 /hr) from the top of the polymerization vessel using a nut pump. ) while performing internal sweeping. Sweeping ended after 30 minutes. At this time, the internal temperature is:
60°C, internal pressure: 0.30Kg/cm 2 -abs., vinyl chloride monomer partial pressure: 0.0001Kg/cm 2 -abs.
比較例 １
実施例１において注水及びジヤケツト加熱を行
なわないで、単にナツシユポンプによる負圧吸引
のみを行なつた場合の30分経過後器内状態は、器
内温度：40℃、器内圧力：0.22Kg／cm2―abs.塩化
ビニルモノマーの分圧：0.15Kg／cm2―abs.であつ
た。Comparative Example 1 In Example 1, when water was not poured and the jacket was heated, and only negative pressure suction was performed using the nut pump, the internal state after 30 minutes was as follows: internal temperature: 40°C, internal pressure: 0.22 Kg/cm 2 -abs.Partial pressure of vinyl chloride monomer: 0.15Kg/cm 2 -abs.
Claims (1)
で重合して得られた重合体スラリーを前記重合器
内から排出した後、前記重合器内に水を注入し、
所望によりこの水を加熱し、この水を蒸発させる
と共に、上部より重合器内ガスを吸引し、重合器
外へ排出し、前記重合器内ガスの吸引排出の間、
重合器内のガスを撹拌するため、重合器内撹拌器
を回転させ、排出されたガスを段階的に凝縮する
ことを特徴とする重合器内に残留するビニル化合
物モノマーの回収方法。 ２ 第１項記載の方法において、前記重合器内ガ
スの吸引量を重合器の単位内容積（m3）当り0.1
〜50Nm3／hrとすることを特徴とする前記方法。 ３ 第１項又は第２項に記載の方法において、前
記重合器内ガスの吸引をナツシユポンプにより行
なうことを特徴とする前記方法。 ４ 第１項ないし第３項のいずれかに記載の方法
において、前記重合器内ガスの吸引の間、前記注
入水の温度を30〜90℃とすることを特徴とする前
記方法。 ５ 第１項ないし第４項のいずれかに記載の方法
において前記ビニル化合物モノマーが、塩化ビニ
ル又はこれを主体とし、これと共重合可能なモノ
マーとの混合物であることを特徴とする前記方
法。[Scope of Claims] 1. A polymer slurry obtained by polymerizing a vinyl compound in an aqueous medium in a polymerization vessel is discharged from the polymerization vessel, and then water is injected into the polymerization vessel,
If desired, the water is heated to evaporate the water, and the gas inside the polymerization vessel is sucked from the upper part and discharged to the outside of the polymerization vessel, and while the gas inside the polymerization vessel is sucked and discharged,
A method for recovering vinyl compound monomers remaining in a polymerization vessel, which comprises rotating an agitator in the polymerization vessel to stir the gas in the polymerization vessel, and condensing the discharged gas in stages. 2 In the method described in item 1, the suction amount of gas in the polymerization vessel is 0.1 per unit internal volume (m 3 ) of the polymerization vessel.
50 Nm 3 /hr. 3. The method according to item 1 or 2, characterized in that the gas inside the polymerization vessel is sucked by a nut pump. 4. The method according to any one of Items 1 to 3, wherein the temperature of the injected water is set at 30 to 90°C during suction of the gas in the polymerization vessel. 5. The method according to any one of items 1 to 4, wherein the vinyl compound monomer is vinyl chloride or a mixture containing vinyl chloride as a main ingredient and a monomer copolymerizable with it.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1596981A JPS57131203A (en) | 1981-02-05 | 1981-02-05 | Recovery of vinyl compound monomer remaining in polymerization vessel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1596981A JPS57131203A (en) | 1981-02-05 | 1981-02-05 | Recovery of vinyl compound monomer remaining in polymerization vessel |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS57131203A JPS57131203A (en) | 1982-08-14 |
| JPH0148283B2 true JPH0148283B2 (en) | 1989-10-18 |
Family
ID=11903535
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1596981A Granted JPS57131203A (en) | 1981-02-05 | 1981-02-05 | Recovery of vinyl compound monomer remaining in polymerization vessel |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS57131203A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5336585A (en) * | 1976-09-16 | 1978-04-04 | Shin Etsu Chem Co Ltd | Production of vinyl chrolide or vinylidene chrolide type polymer |
-
1981
- 1981-02-05 JP JP1596981A patent/JPS57131203A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5336585A (en) * | 1976-09-16 | 1978-04-04 | Shin Etsu Chem Co Ltd | Production of vinyl chrolide or vinylidene chrolide type polymer |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS57131203A (en) | 1982-08-14 |
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