JPH08134012A - Equipment for removing high-boiling-point impurities in oxidation reaction product gas - Google Patents
Equipment for removing high-boiling-point impurities in oxidation reaction product gasInfo
- Publication number
- JPH08134012A JPH08134012A JP27952394A JP27952394A JPH08134012A JP H08134012 A JPH08134012 A JP H08134012A JP 27952394 A JP27952394 A JP 27952394A JP 27952394 A JP27952394 A JP 27952394A JP H08134012 A JPH08134012 A JP H08134012A
- Authority
- JP
- Japan
- Prior art keywords
- boiling
- reaction product
- product gas
- point
- impurities
- 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.)
- Pending
Links
- 239000012535 impurity Substances 0.000 title claims abstract description 71
- 239000007795 chemical reaction product Substances 0.000 title claims abstract description 37
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 12
- 238000009835 boiling Methods 0.000 claims abstract description 28
- 238000000151 deposition Methods 0.000 claims abstract description 22
- 238000001556 precipitation Methods 0.000 claims abstract description 21
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 15
- 230000008021 deposition Effects 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 10
- 230000003197 catalytic effect Effects 0.000 claims abstract description 9
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 230000001376 precipitating effect Effects 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 42
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 10
- 238000001816 cooling Methods 0.000 description 8
- 238000005192 partition Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000012856 packing Methods 0.000 description 5
- 239000012071 phase Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000012670 alkaline solution Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000003517 fume Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- STNJBCKSHOAVAJ-UHFFFAOYSA-N Methacrolein Chemical compound CC(=C)C=O STNJBCKSHOAVAJ-UHFFFAOYSA-N 0.000 description 1
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- ZWLPBLYKEWSWPD-UHFFFAOYSA-N o-toluic acid Chemical compound CC1=CC=CC=C1C(O)=O ZWLPBLYKEWSWPD-UHFFFAOYSA-N 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007039 two-step reaction Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
(57)【要約】
【目的】 炭素数４の化合物を気相接触酸化反応を行う
ことにより得られるメタクリル酸を含有する反応生成ガ
ス中から高沸点不純物を選択的に析出除去するための装
置を提供する。
【構成】 炭素数４の化合物の気相接触酸化反応で得ら
れるメタクリル酸を含有する反応生成ガスを凝縮させ、
得られる凝縮液からメタクリル酸を捕集する方法におい
て使用するための高沸点不純物除去装置であり、かかる
高沸点不純物除去装置が反応器から流出する反応生成ガ
スの導管に接触しており、高沸点不純物を選択的に析出
させるための高沸点不純物析出帯を２組以上、析出した
高沸点不純物を洗浄するための洗浄設備を２組以上、か
かる洗浄設備を備えた前記高沸点不純物析出帯収納用ハ
ウジングを２組以上、及び前記高沸点不純物析出帯を移
動させるための駆動装置から構成された高沸点不純物除
去装置。
(57) [Summary] [Purpose] An apparatus for selectively depositing and removing high boiling impurities from a reaction product gas containing methacrylic acid obtained by carrying out a gas phase catalytic oxidation reaction of a compound having 4 carbon atoms. provide. [Structure] A reaction product gas containing methacrylic acid obtained by a gas phase catalytic oxidation reaction of a compound having 4 carbon atoms is condensed,
A high-boiling-point impurity removing device for use in the method of collecting methacrylic acid from the obtained condensate, and the high-boiling-point impurity removing device is in contact with the conduit of the reaction product gas flowing out from the reactor, and has a high boiling point. Two or more sets of high-boiling-point impurity precipitation zones for selectively precipitating impurities, two or more sets of cleaning equipment for cleaning the precipitated high-boiling-point impurities, and a storage facility for storing the high-boiling-point impurity precipitation zones equipped with such cleaning equipment A high-boiling-point impurity removing device comprising two or more sets of housings and a driving device for moving the high-boiling-point impurity deposition zone.
Description
【０００１】[0001]
【産業上の利用分野】本発明は、炭素数４の化合物を気
相接触酸化反応を行うことにより得られるメタクリル酸
を含有する反応生成ガス中から高沸点不純物を選択的に
析出除去し、反応生成ガスの冷却凝縮工程以降のプロセ
スに発生するトラブルを解消するための装置に関する。FIELD OF THE INVENTION The present invention relates to a reaction product gas containing methacrylic acid, which is obtained by subjecting a compound having 4 carbon atoms to a gas phase catalytic oxidation reaction, to selectively precipitate and remove high-boiling-point impurities from the reaction product gas. The present invention relates to an apparatus for eliminating troubles that occur in processes after the cooling and condensation process of generated gas.
【０００２】[0002]
【従来の技術】炭素数４の化合物を水蒸気の存在下に分
子状酸素で１段または２段の反応で接触酸化して得られ
るメタクリル酸を含む反応生成ガスを冷却凝縮して得ら
れる該ガスの凝縮液中には、反応で副生する種々の不純
物が存在する。これらの不純物としては、例えば酢酸、
アクロレイン、アセトアルデヒド、メタクロレイン、ア
クリル酸、さらに微量のテレフタル酸、トルイル酸、安
息香酸等の芳香族化合物やタ−ル状物質等が挙げられ
る。2. Description of the Related Art A gas produced by cooling and condensing a reaction product gas containing methacrylic acid obtained by catalytically oxidizing a compound having 4 carbon atoms with molecular oxygen in a one- or two-step reaction in the presence of water vapor. In the condensate of, there are various impurities by-produced in the reaction. Examples of these impurities include acetic acid,
Examples thereof include acrolein, acetaldehyde, methacrolein, acrylic acid, and a trace amount of an aromatic compound such as terephthalic acid, toluic acid, benzoic acid, and a tar-like substance.
【０００３】これらの不純物の中でも比較的高融点であ
る多塩基性有機酸、特にテレフタル酸は反応生成ガスの
冷却工程（一般に急冷塔が用いられる。）で反応生成ガ
スの凝縮液と非凝縮ガスを得る際に、かかる凝縮液への
溶解度が低いために配管や塔壁等に析出し閉塞を起こし
たり、また反応生成ガスが冷却されるときに微細な粒
子、いわゆるヒュ−ムを生成するため、該ヒュ−ムの非
凝縮ガスからの分離に困難を来し、以後の工程で種々の
トラブルの原因となる。Among these impurities, a polybasic organic acid having a relatively high melting point, particularly terephthalic acid, is used in a reaction product gas cooling step (a quenching tower is generally used) in the reaction product gas condensate and non-condensate gas. When the reaction product gas is cooled, the solubility in the condensate is low, so that it precipitates on the pipe or tower wall to cause blockage, and when the reaction product gas is cooled, it produces fine particles, so-called fumes. However, separation of the fumes from the non-condensable gas becomes difficult, and causes various troubles in the subsequent steps.
【０００４】一方、メタクリル酸を含む反応生成ガスの
凝縮液中にわずかに溶解したテレフタル酸は、次の溶剤
を用いた凝縮液からのメタクリル酸の抽出工程で溶剤中
へのテレフタル酸の溶解度が低下して系内に析出し、配
管等の詰まりの原因となり、上記抽出工程を含むメタク
リル酸製造工程の連続運転の大きな支障となっている。On the other hand, terephthalic acid slightly dissolved in the condensate of the reaction product gas containing methacrylic acid has a solubility of terephthalic acid in the solvent in the extraction step of methacrylic acid from the condensate using the following solvent. It lowers and precipitates in the system, causing clogging of pipes and the like, which is a great obstacle to continuous operation of the methacrylic acid production process including the extraction process.
【０００５】これらのトラブルを解決するための方法と
して様々なものが提案されている。例えば、特開昭５８
−５２２３９号には反応生成ガスの冷却工程前に高沸点
不純物のみを選択的に捕集する方法が提案されている。
この方法では反応器と凝縮器の間に捕集器を設置し、連
続または断続的に固体として得られる高沸点不純物を系
外に取り出している。Various methods have been proposed as methods for solving these problems. For example, JP-A-58
No. 52239 proposes a method of selectively collecting only high-boiling-point impurities before the step of cooling the reaction product gas.
In this method, a collector is installed between the reactor and the condenser to continuously or intermittently take out high-boiling impurities obtained as a solid from the system.
【０００６】しかしながら、かかる方法は生産量の少な
いパイロットプラントへの適用は可能であるが、生産量
が数万トン／年以上のプラントには適用が難しい。その
理由としては炭素数４の化合物を気相接触酸化反応を行
ってメタクリル酸を得る方法では反応器から出てくる反
応生成ガス中のメタクルリ酸含有量が数％程度で、かつ
高温度であるため工業的に有利な規模にまで生産量を拡
大すると、反応生成ガスが通る配管はその後のメタクリ
ル酸凝縮液の配管等に比べて非常に太いものにせざるを
得ない。However, although such a method can be applied to a pilot plant having a small production amount, it is difficult to apply it to a plant having a production amount of tens of thousands tons / year or more. The reason is that in the method of obtaining methacrylic acid by subjecting a compound having 4 carbon atoms to a gas phase catalytic oxidation reaction, the content of methacrylic acid in the reaction product gas discharged from the reactor is about several% and the temperature is high. Therefore, when the production amount is expanded to an industrially advantageous scale, the pipe through which the reaction product gas passes must be extremely thick as compared with the subsequent pipe for the methacrylic acid condensate.
【０００７】このような太く、かつ高温度の配管中に切
り替え用の弁や、回転摺動部分を有するような構造は非
現実的であり、工業的安全運転の観点からも好ましくな
い。仮にかかる構造のものを製造する場合には過大な費
用を伴うものであり現実的ではない。A structure having such a switching valve and a rotary sliding portion in a thick and high-temperature pipe is unrealistic and is not preferable from the viewpoint of industrial safe operation. If such a structure is manufactured, it is not realistic because it involves an excessive cost.
【０００８】また、ガス系での閉塞によるトラブルが起
きた場合、液系のようにタンク等に一時貯蔵するといっ
た処置はできず、プラント自体を休止せざるを得なく、
万全の対策を考慮した装置が要求される。Further, when a trouble occurs due to blockage in the gas system, it is impossible to temporarily store it in a tank or the like like a liquid system, and the plant itself must be stopped.
A device that takes all possible measures into consideration is required.
【０００９】[0009]
【発明が解決しようとする課題】本発明は、上述した如
き問題点を有さない、酸化反応生成ガス中のテレフタル
酸等の高沸点不純物を除去する装置を提供することを目
的としている。SUMMARY OF THE INVENTION It is an object of the present invention to provide a device for removing high boiling impurities such as terephthalic acid in the oxidation reaction product gas, which does not have the above-mentioned problems.
【００１０】[0010]
【発明が解決しようとする課題】本発明は、炭素数４の
化合物の気相接触酸化反応で得られるメタクリル酸を含
有する反応生成ガスを凝縮させ、得られる凝縮液からメ
タクリル酸を捕集する方法において使用するための高沸
点不純物除去装置であり、該除去装置が反応器から流出
する反応生成ガスの導管に接触しており、高沸点不純物
を選択的に析出させるための高沸点不純物析出帯が２組
以上、析出した高沸点不純物を洗浄するための洗浄設備
が２組以上、前記洗浄設備を備えた前記高沸点不純物析
出帯収納用のハウジングが２組以上、及び前記高沸点不
純物析出帯を移動させるための駆動装置から構成される
ことを特徴とする高沸点不純物除去装置を要旨とするも
のである。DISCLOSURE OF THE INVENTION According to the present invention, a reaction product gas containing methacrylic acid obtained by a gas phase catalytic oxidation reaction of a compound having 4 carbon atoms is condensed and methacrylic acid is collected from the obtained condensate. A high-boiling-point impurity removing device for use in a method, wherein the removing device is in contact with a conduit of a reaction product gas flowing out from a reactor, and a high-boiling-point impurity deposition zone for selectively precipitating high-boiling-point impurities. 2 or more sets, 2 or more sets of cleaning equipment for cleaning the precipitated high boiling point impurities, 2 or more sets of housings for storing the high boiling point impurity deposition zones equipped with the cleaning equipment, and the high boiling point impurity deposition zones A high-boiling-point impurity removing device is characterized in that it comprises a driving device for moving the.
【００１１】以下、図面に基づいて本発明を詳細に説明
する。第１図は本発明の高沸点不純物除去装置の外観図
である。基本的構造は反応生成ガスを導入する導管の周
りに２組以上の駆動式の高沸点不純物析出帯を付した構
造をしている。図には示されていない接触酸化工程によ
って得られたメタクリル酸を含む反応生成ガスは導管１
によって高沸点不純物析出装置に導入され、その後導管
２を通って、図には示されていないが反応生成ガスを冷
却凝縮するための凝縮器へと導かれる。The present invention will be described in detail below with reference to the drawings. FIG. 1 is an external view of the high boiling point impurity removing apparatus of the present invention. The basic structure is such that two or more sets of driven high-boiling-point impurity precipitation zones are provided around the conduit for introducing the reaction product gas. The reaction product gas containing methacrylic acid obtained by the catalytic oxidation step not shown in the figure
Is introduced into the high-boiling-point impurity depositing apparatus and then led through the conduit 2 to a condenser (not shown) for cooling and condensing the reaction product gas.
【００１２】次に第２図により高沸点不純物析出装置の
詳細について説明する。高沸点不純物析出装置は高沸点
不純物が析出するための２組以上の高沸点不純物析出帯
と、これらを収納するハウジングで構成されており、ハ
ウジング内から反応ガスが漏れないように密封構造とな
っている。Next, the details of the high boiling point impurity depositing apparatus will be described with reference to FIG. The high-boiling-point impurity depositing device is composed of two or more pairs of high-boiling-point impurity depositing zones for depositing high-boiling-point impurities and a housing that houses them, and has a sealed structure to prevent reaction gas from leaking from inside the housing. ing.
【００１３】第２図は２組の高沸点不純物析出帯を設け
た場合であるが、高沸点不純物析出帯は２組以上でも良
い。それぞれの部屋をＡ、Ｂ及びＣとすると、Ｂは反応
生成ガスが通り、高沸点不純物を析出させる部分であ
り、Ａ及びＣは反応生成ガスが入り込まないように仕切
り板４’、５及びパッキング８、８’、９及び９’によ
りシ−ルされている。第２図の場合、Ｃは析出した不純
物を洗浄、乾燥するための部屋、Ａは収納されていた析
出帯が反応生成ガスの導管内に移動した状態であり、空
の部屋となっている。Although FIG. 2 shows the case where two sets of high boiling point impurity precipitation zones are provided, two or more sets of high boiling point impurity precipitation zones may be provided. Letting A, B and C be the respective chambers, B is a portion through which the reaction product gas passes and deposits high boiling impurities, and A and C are partition plates 4 ', 5 and packing so that the reaction product gas does not enter. Sealed by 8, 8 ', 9 and 9'. In the case of FIG. 2, C is a room for cleaning and drying the precipitated impurities, and A is an empty room in which the contained deposition zone is moved into the reaction product gas conduit.
【００１４】高沸点不純物析出帯の構造は反応生成ガス
と接触する部分の表面積を大きくしたものであり、反応
生成ガスの流れを妨げない構造であれば特に限定されな
いが、その一例としては第２図の３に示したような熱交
換に一般に用いられているフィンのついた導管を仕切り
板４及び４’の表面に配置したものが挙げられる。The structure of the high-boiling-point impurity precipitation zone is formed by increasing the surface area of the portion in contact with the reaction product gas, and is not particularly limited as long as it does not impede the flow of the reaction product gas. As an example, a finned conduit generally used for heat exchange as shown in FIG. 3 is arranged on the surfaces of the partition plates 4 and 4 '.
【００１５】高沸点不純物の析出はバルブ６、導管７を
通して析出帯を構成する各フィン付き導管に供給される
スチ−ムによって温度をコントロ−ルすることにより行
われる。また、フィンの表面温度としては高沸点不純物
のみを選択的に析出するための温度として反応生成ガス
の高沸点不純物析出装置での操作圧力における露点以上
であることが好ましい。Deposition of high-boiling-point impurities is carried out by controlling the temperature by means of the steam supplied to each finned conduit constituting the precipitation zone through the valve 6 and the conduit 7. The surface temperature of the fins is preferably a temperature for selectively precipitating only high-boiling-point impurities, which is equal to or higher than the dew point of the reaction product gas at the operating pressure in the high-boiling-point impurity depositing apparatus.
【００１６】以下に本発明の装置の代表的な運転方法に
ついて説明する。運転中は上述したとおり、反応生成ガ
スが通り、高沸点不純物の析出が行われる部屋と、析出
した高沸点不純物を洗浄、乾燥する部屋に分けられる。
なお、この二つの部屋のシ−ルは第２図に示すようにパ
ッキン８に中央仕切り板５を油圧シリンダ−駆動装置１
０、１０’で押し当てることで達成できる。A typical operation method of the apparatus of the present invention will be described below. As described above, during operation, the reaction product gas passes through and is divided into a room in which high boiling point impurities are deposited and a room in which the deposited high boiling point impurities are washed and dried.
In addition, as shown in FIG. 2, the seals of the two chambers are such that a packing 8 is provided with a central partition plate 5 and a hydraulic cylinder drive unit 1.
It can be achieved by pressing 0, 10 '.
【００１７】高沸点不純物析出帯の切り替え時期は１１
及び１１’の高沸点不純物析出帯前後に取り付けられた
圧力計によって決定され、析出物の増加により圧力損失
が一定値を超えると油圧シリンダ−駆動装置１０、１
０’に連動して高沸点不純物析出帯が移動し、高沸点不
純物の析出した析出帯が反応生成ガスの通過部から外側
に出され、もう１組の高沸点不純物析出帯が導管内側に
導入される。切り替えはＡ及びＣのハウジング内に導管
１２、１２’を通して不活性ガスまたは反応生成ガスの
一部をパ−ジし、温度、圧力をＢの部分と同じにするこ
とによって問題なく行うことができる。The switching time of the high boiling point impurity precipitation zone is 11
And 11 ', which are determined by pressure gauges installed before and after the high-boiling-point impurity precipitation zone, and when the pressure loss exceeds a certain value due to an increase in the precipitation, the hydraulic cylinder-driving device 10, 1
The high-boiling-point impurity precipitation zone moves in conjunction with 0 ', the precipitation zone where the high-boiling-point impurities are precipitated is discharged outside from the passage of the reaction product gas, and another set of high-boiling-point impurity precipitation zones is introduced inside the conduit. To be done. The switching can be carried out without problems by purging a part of the inert gas or the reaction product gas through the conduits 12 and 12 'in the housings A and C so that the temperature and the pressure are the same as those in the part B. .
【００１８】第２図の状態から高沸点不純物析出帯の切
替を行った状態を第３図に示す。この時反応生成ガス通
過部から外側に出された高沸点不純物析出帯上に析出し
た高沸点不純物は、再び導管内側に導入されるまでにア
ルカリ溶液等により洗浄される。洗浄の方法は特に限定
されないが、切り替え終了後に１２’の導管からアンモ
ニア水溶液等のアルカリ溶液を導入し、１３’の噴出口
により析出帯全体にかけて溶解、洗浄し、１４’の導管
により排出する方法等が挙げられる。さらに洗浄後のア
ルカリ溶液を排出した後は導管１２’より不活性ガスを
パ−ジし、フィン付き導管にスチ−ムを流し、高沸点不
純物析出帯を昇温、乾燥して次の交換に備えればよい。FIG. 3 shows a state in which the high boiling point impurity deposition zone is switched from the state of FIG. At this time, the high-boiling-point impurities deposited on the high-boiling-point impurity deposition zone that are discharged outside from the reaction product gas passage are washed with an alkaline solution or the like before being introduced inside the conduit again. The washing method is not particularly limited, but after the switching is completed, an alkaline solution such as an aqueous ammonia solution is introduced from the 12 'conduit, dissolved and washed throughout the deposition zone by the 13' jet outlet, and discharged by the 14 'conduit. Etc. After discharging the alkaline solution after washing, an inert gas is purged from the conduit 12 'and a steam is flown through the finned conduit to heat and dry the high boiling point impurity deposition zone for the next exchange. Be prepared.
【００１９】[0019]
【実施例】以下、実施例により本発明を具体的に説明す
る。 実施例１ タ−シャリ−ブタノ−ルの接触気相酸化法によるメタク
リル酸製造プラントにおいて、酸化反応器を出た反応生
成ガスを第１図に示す高沸点不純物析出装置を設けた配
管を通し、次の冷却工程へ導入した。The present invention will be described below in detail with reference to examples. Example 1 In a methacrylic acid production plant by catalytic vapor phase oxidation of tertiary butanol, the reaction product gas exiting the oxidation reactor was passed through a pipe provided with a high-boiling point impurity depositing apparatus shown in FIG. It was introduced into the next cooling step.
【００２０】高沸点不純物析出帯の表面温度を２００℃
として１ケ月の連続運転を行った。高沸点不純物析出帯
前後の圧力損失は１５日間で０．１ｋｇ／ｃｍ2 上昇
し、この時点で高沸点不純物析出帯の切り替えを行った
ところ、良好に行うことができた。また、運転終了後に
析出した高沸点不純物をアンモニア水溶液の洗浄によっ
て殆ど全量を洗い流すことができた。The surface temperature of the high boiling point impurity precipitation zone is 200 ° C.
As a result, continuous operation was performed for one month. The pressure loss before and after the high-boiling-point impurity precipitation zone increased by 0.1 kg / cm 2 in 15 days, and when the high-boiling-point impurity precipitation zone was switched at this point, the high-boiling-point impurity precipitation zone was satisfactorily performed. Further, almost all the high boiling point impurities deposited after the operation could be washed away by washing the aqueous ammonia solution.
【００２１】比較例１ 実施例１と同じガス組成の反応生成ガスを高沸点不純物
析出装置を通さずに冷却工程に導入したところ、凝縮器
導入部に高沸点不純物の析出が起こり、２日間で運転不
能となった。Comparative Example 1 When the reaction product gas having the same gas composition as in Example 1 was introduced into the cooling step without passing through the high-boiling point impurity depositing apparatus, precipitation of high-boiling point impurities occurred in the condenser introducing part, and the reaction was continued for 2 days. It became impossible to operate.
【００２２】[0022]
【発明の効果】本発明は、上述した如き構成の装置から
なるため、この装置に炭素数４の化合物を気相接触酸化
反応を行うことにより得られるメタクリル酸を含有する
反応生成ガスを導入することにより該ガス中から高沸点
不純物を選択的に析出除去し、反応生成ガスの冷却凝縮
工程以降のプロセスに発生しがちなトラブルを解消する
ことができる等の優れた効果を奏する。EFFECTS OF THE INVENTION Since the present invention comprises an apparatus having the above-mentioned constitution, a reaction product gas containing methacrylic acid obtained by carrying out a gas phase catalytic oxidation reaction of a compound having 4 carbon atoms is introduced into this apparatus. By doing so, high boiling impurities are selectively deposited and removed from the gas, and excellent effects such as troubles that tend to occur in the process after the cooling and condensation process of the reaction product gas can be solved.
【図１】本発明の高沸点不純物除去装置の外観図であ
る。FIG. 1 is an external view of a high boiling point impurity removing device of the present invention.
【図２】２組の高沸点不純物析出帯を設けた高沸点不純
物除去装置の断面図である。FIG. 2 is a cross-sectional view of a high-boiling-point impurity removing device provided with two sets of high-boiling-point impurity precipitation zones.
【図３】第２図の状態から高沸点不純物析出帯の切り替
えを行った状態の高沸点不純物除去装置の断面図であ
る。FIG. 3 is a cross-sectional view of the high-boiling-point impurity removing device in a state where the high-boiling-point impurity deposition zone is switched from the state of FIG.
１ 導管 ２ 導管 ３ フィン付き導管 ４ 仕切り板 ４’ 仕切り板 ５ 中央仕切り板 ６ バルブ ７ 導管 ８ パッキング ８’ パッキング ９ パッキング １０ 油圧シリンダ−駆動装置 １０’ 油圧シリンダ−駆動装置 １１ 圧力計 １２ 導管 １２’ 導管 １３ 噴出口 １４ 導管 １４’ 導管 1 conduit 2 conduit 3 finned conduit 4 partition plate 4'partition plate 5 central partition plate 6 valve 7 conduit 8 packing 8'packing 9 packing 10 hydraulic cylinder-driving device 10 'hydraulic cylinder-driving device 11 pressure gauge 12 conduit 12' Conduit 13 Jet port 14 Conduit 14 'Conduit
Claims (1)
得られるメタクリル酸を含有する反応生成ガスを凝縮さ
せ、得られる凝縮液からメタクリル酸を捕集する方法に
おいて使用するための高沸点不純物除去装置であり、該
除去装置が反応器から流出する反応生成ガスの導管に接
触しており、高沸点不純物を選択的に析出させるための
高沸点不純物析出帯が２組以上、析出した高沸点不純物
を洗浄するための洗浄設備が２組以上、前記洗浄設備を
備えた前記高沸点不純物析出帯収納用のハウジングが２
組以上、及び前記高沸点不純物析出帯を移動させるため
の駆動装置から構成されることを特徴とする高沸点不純
物除去装置。1. A high boiling point for use in a method of condensing a reaction product gas containing methacrylic acid obtained by a gas phase catalytic oxidation reaction of a compound having 4 carbon atoms, and collecting methacrylic acid from the obtained condensate. An impurity removing device, the removing device is in contact with a conduit of a reaction product gas flowing out from the reactor, and two or more sets of high boiling point impurity deposition zones for selectively depositing high boiling point impurities are provided. There are two or more sets of cleaning equipment for cleaning the impurities in the boiling point, and two housings for accommodating the high-boiling-point impurity precipitation zone equipped with the cleaning equipment.
An apparatus for removing high-boiling-point impurities, characterized by comprising at least one set and a driving device for moving the high-boiling-point impurity precipitation zone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27952394A JPH08134012A (en) | 1994-11-14 | 1994-11-14 | Equipment for removing high-boiling-point impurities in oxidation reaction product gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27952394A JPH08134012A (en) | 1994-11-14 | 1994-11-14 | Equipment for removing high-boiling-point impurities in oxidation reaction product gas |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08134012A true JPH08134012A (en) | 1996-05-28 |
Family
ID=17612215
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27952394A Pending JPH08134012A (en) | 1994-11-14 | 1994-11-14 | Equipment for removing high-boiling-point impurities in oxidation reaction product gas |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08134012A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004022518A1 (en) * | 2002-09-03 | 2004-03-18 | Mitsubishi Chemical Corporation | Process for producing (meth)acrylic acid compound |
| JP2005298384A (en) * | 2004-04-09 | 2005-10-27 | Asahi Kasei Chemicals Corp | Method for cooling reaction gas containing (meth) acrylic acid and / or (meth) acrolein |
| US7279076B2 (en) | 2001-12-21 | 2007-10-09 | Mitsubishi Chemical Corporation | Apparatus and method for handling easily polymerizable substance, apparatus for extracting liquid from apparatus under reduced pressure, and process for producing easily polymerizable substance |
-
1994
- 1994-11-14 JP JP27952394A patent/JPH08134012A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7279076B2 (en) | 2001-12-21 | 2007-10-09 | Mitsubishi Chemical Corporation | Apparatus and method for handling easily polymerizable substance, apparatus for extracting liquid from apparatus under reduced pressure, and process for producing easily polymerizable substance |
| WO2004022518A1 (en) * | 2002-09-03 | 2004-03-18 | Mitsubishi Chemical Corporation | Process for producing (meth)acrylic acid compound |
| US7166741B2 (en) | 2002-09-03 | 2007-01-23 | Mitsubishi Chemical Corporation | Process for producing (meth) acrylic acid compound |
| JP2005298384A (en) * | 2004-04-09 | 2005-10-27 | Asahi Kasei Chemicals Corp | Method for cooling reaction gas containing (meth) acrylic acid and / or (meth) acrolein |
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