JPS6132300B2 - - Google Patents
Info
- Publication number
- JPS6132300B2 JPS6132300B2 JP53117569A JP11756978A JPS6132300B2 JP S6132300 B2 JPS6132300 B2 JP S6132300B2 JP 53117569 A JP53117569 A JP 53117569A JP 11756978 A JP11756978 A JP 11756978A JP S6132300 B2 JPS6132300 B2 JP S6132300B2
- Authority
- JP
- Japan
- Prior art keywords
- acetic acid
- terephthalic acid
- inert gas
- container
- acid
- 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
Links
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 171
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 126
- 239000011261 inert gas Substances 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 23
- 239000007789 gas Substances 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 239000012535 impurity Substances 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229920000728 polyester Polymers 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- -1 polyethylene terephthalate Polymers 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- GOUHYARYYWKXHS-UHFFFAOYSA-N 4-formylbenzoic acid Chemical compound OC(=O)C1=CC=C(C=O)C=C1 GOUHYARYYWKXHS-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- LPNBBFKOUUSUDB-UHFFFAOYSA-N p-toluic acid Chemical compound CC1=CC=C(C(O)=O)C=C1 LPNBBFKOUUSUDB-UHFFFAOYSA-N 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000005711 Benzoic acid Substances 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000003134 recirculating effect Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
【発明の詳細な説明】
本発明は酢酸を含有するテレフタル酸（粉体）
を容器から容器へ気力輸送によつて輸送する方法
に関するものである。[Detailed description of the invention] The present invention provides terephthalic acid (powder) containing acetic acid.
The present invention relates to a method for transporting from container to container by pneumatic transport.
テレフタル酸は繊維、フイルム、成型品等の材
料であるポリエチレンテレフタレート、ポリプチ
レンテレフタレート等のポリエステルの原料とし
て大量に使用されている粉体であり、それを連続
的に容器から容器へ輸送する場合、セメント、石
灰、アルミナ、穀類のような粉粒体の輸送に広く
用いられている気力輸送によるのが通常である。
気力輸送は設置が容易で既存の複雑な構造物など
の障害物にわずらわされることなく配管でき、密
閉系であり飛散のおそれがないなどの利点はある
が、帯電性の粉体では粉塵爆発の危険がある。し
たがつてテレフタル酸の気力輸送の場合も粉塵爆
発を防止するため窒素、炭酸ガスなどの不活性ガ
スが用いられる。またテレフタル酸の気力輸送に
際し容器内での粉体テレフタル酸を流動化させる
ため窒素などの不活性ガスの吹き込みが行われ
る。テレフタル酸の気力輸送および流動化に使用
される不活性ガスは高価であり空気中に排出され
ることなく循環使用されるのが通常である。 Terephthalic acid is a powder that is used in large quantities as a raw material for polyesters such as polyethylene terephthalate and polybutylene terephthalate, which are materials for fibers, films, molded products, etc. When it is continuously transported from container to container, Usually, pneumatic transport is used, which is widely used for transporting granular materials such as cement, lime, alumina, and grains.
Pneumatic transport has the advantage of being easy to install, piping can be done without being bothered by obstacles such as existing complex structures, and is a closed system so there is no risk of scattering. Risk of dust explosion. Therefore, in the case of pneumatic transport of terephthalic acid, an inert gas such as nitrogen or carbon dioxide gas is used to prevent dust explosions. Furthermore, during pneumatic transport of terephthalic acid, inert gas such as nitrogen is blown into the container to fluidize the powdered terephthalic acid within the container. The inert gas used for pneumatic transportation and fluidization of terephthalic acid is expensive and is usually recycled without being discharged into the air.
テレフタル酸は多くはパラキシレンの酸化によ
つて製造され、その製造方法は種々ある。テレフ
タル酸中に存在し、ポリエステルの色調などの品
質に悪影響を与える微量の不純分を除くための精
製工程もこの酸化の触媒、反応条件等によつて含
まれる不純分が異なることによりいろいろ提案が
なされている。たとえば酢酸中で酸化反応により
製造されたテレフタル酸を酢酸水溶液中で懸濁状
態において洗浄し、遠心分離、乾燥する方法（特
公昭51−46098）や、テレフタル酸を酢酸と少量
の硝酸を含む水溶液中で懸濁状態で加熱処理後、
濾別、洗浄、乾燥する方法（特公昭51−45579、
特公昭51−46099）や、テレフタル酸に酢酸をふ
りかけ洗浄、乾燥する方法（特開昭52−89637）
などがある。かかる精製、乾燥工程を経たテレフ
タル酸は微量の酢酸、４−カルボキシベンズアル
デヒド、ｐ−トルイル酸、安息香酸などを含有し
ているが、そのままポリエステル製造原料として
使用され、高品位のポリエステルが得られてい
る。しかるに本発明者らはかかる原料テレフタル
酸とグリコールとから長期にわたつてひきつづき
ポリエステルを製造していると、原料テレフタル
酸の不純分量に変化がないにもかかわらず、得ら
れるポリマー品質、特にポリマーの色調にむらが
発生することを経験した。本発明者らはこの原因
を追求した結果、テレフタル酸を気力輸送するに
際しテレフタル酸から揮発した不活性ガス中の酢
酸が凝縮してドレンとなつた時このドレン（液
滴）にテレフタル酸中の不純物が集中し、その輸
送時のテレフタル酸に混入してポリマーの色調に
むらを生じていることを見い出した。 Terephthalic acid is mostly produced by oxidizing paraxylene, and there are various methods for producing it. Various proposals have been made regarding the purification process to remove trace amounts of impurities that exist in terephthalic acid and adversely affect the color tone and other quality of polyester, as the impurities contained in this oxidation catalyst and reaction conditions vary. being done. For example, there is a method in which terephthalic acid produced by an oxidation reaction in acetic acid is washed in suspension in an acetic acid aqueous solution, centrifuged, and dried (Japanese Patent Publication No. 51-46098), and terephthalic acid is prepared in an aqueous solution containing acetic acid and a small amount of nitric acid. After heat treatment in suspension in
Method of filtering, washing, and drying (Special Publication No. 51-45579,
(Japanese Patent Publication No. 51-46099) and method of washing and drying by sprinkling acetic acid on terephthalic acid (Japanese Patent Publication No. 52-89637)
and so on. Terephthalic acid that has gone through this purification and drying process contains trace amounts of acetic acid, 4-carboxybenzaldehyde, p-toluic acid, benzoic acid, etc., but it can be used as a raw material for polyester production as it is, and high-quality polyester can be obtained. There is. However, when the present inventors continued to produce polyester from such raw materials terephthalic acid and glycol over a long period of time, the resulting polymer quality, especially the polymer I experienced uneven color tone. The present inventors investigated the cause of this problem and found that when acetic acid in the inert gas that volatilized from terephthalic acid condensed and became drain when terephthalic acid was pneumatically transported, the condensate (droplets) contained in the terephthalic acid It was discovered that impurities were concentrated and mixed into the terephthalic acid during transportation, causing uneven color tone of the polymer.
すなわち酢酸を含む溶液で精製されたテレフタ
ル酸は乾燥後であつてもいくらかの酢酸を含有し
ている。テレフタル酸粉体に酢酸を含まぬ窒素な
どのガスを長時間必要なだけ通気すると、通気し
たガス中にはテレフタル酸から脱離した酢酸が含
まれる。この通気したガスをガス吸収器にてトラ
ツプし、吸収液中の酢酸量をガスクロマトグラフ
によつて測定すると、通気時間約100時間でテレ
フタル酸から脱離しおわることがわかる。そして
その結果テレフタル酸の乾燥条件によつて変わる
がテレフタル酸に対し20ppm以上数百ppm（重
量比）の酢酸を含有していることがわかつた。い
ずれにしても酢酸を含有する粉状テレフタル酸を
容器から容器へ窒素のような不活性ガスを再循環
して密閉系で気力輸送するに際しテレフタル酸中
の酢酸がテレフタル酸に対し20ppm以上数百
ppm（重量比）不活性ガス中に揮発するので、
循環再使用不活性ガス中の酢酸濃度が次第に増加
する。 That is, terephthalic acid purified in a solution containing acetic acid contains some acetic acid even after drying. When acetic acid-free gas such as nitrogen is aerated through terephthalic acid powder for as long as necessary, the aerated gas contains acetic acid released from the terephthalic acid. When this vented gas is trapped in a gas absorber and the amount of acetic acid in the absorbed liquid is measured using a gas chromatograph, it is found that the acetic acid is completely desorbed from the terephthalic acid after about 100 hours of venting. As a result, it was found that the acetic acid content was 20 ppm to several hundred ppm (weight ratio) to terephthalic acid, although it varied depending on the drying conditions of the terephthalic acid. In any case, when powdered terephthalic acid containing acetic acid is pneumatically transported from container to container in a closed system by recirculating an inert gas such as nitrogen, the acetic acid in the terephthalic acid is 20 ppm or more than several hundred ppm relative to terephthalic acid.
ppm (weight ratio) as it volatilizes in inert gas,
The acetic acid concentration in the recycled inert gas gradually increases.
テレフタル酸の気力輸送においては、気力輸送
時に輸送停止時との不活性ガスの温度を比較する
と、気力輸送時に粉状テレフタル酸と配管との摩
擦熱によつて輸送停止時と比べて10〜20℃不活性
ガスの温度が高くなることがある。また夜間には
外気温の低下と共に外気温にさらされる循環再使
用不活性ガスの温度が低下する。かかる温度変化
によつて循環再使用不活性ガス中の酢酸が凝縮し
ドレンを生じ、輸送配管中のドレンが妨害物とな
り気力輸送中のテレフタル酸の配管詰りが生じ
る。またテレフタル酸を貯蔵した容器中のテレフ
タル酸の流動化のため常時間欠的に不活性ガスを
吹き込んでいても、容器の下部吐出口から酢酸を
含有した不活性ガスが吹上がり、その酢酸によつ
て容器下部の粉状テレフタル酸が湿潤化し落下不
調となり、容器吐出口を解体して掃除することが
必要となる。酢酸が凝縮したドレンを配管中から
採取し、これをテレフタル酸に約100ppm（重量
比）混ぜエチレングリコールとエステル化し、重
縮合反応を行うと得られたポリエチレンテレフタ
レートに色調異常が発生した。したがつて酢酸が
凝縮したドレンには集中的にテレフタル酸中の不
純分が集まり、それが気力輸送時にテレフタル酸
に部分的に混入しポリマーの品質低下、特にポリ
マーの色調のむらを生じるものと推定される。 In pneumatic transport of terephthalic acid, when comparing the temperature of the inert gas during pneumatic transport with when transport is stopped, it is found that the temperature of the inert gas during pneumatic transport is 10 to 20% lower than when transport is stopped due to frictional heat between powdered terephthalic acid and piping. °C The temperature of the inert gas may become high. Furthermore, at night, as the outside temperature drops, the temperature of the reused inert gas exposed to the outside temperature also drops. Due to such a temperature change, the acetic acid in the reused inert gas condenses to form a drain, and the drain in the transportation piping becomes an obstruction, causing the terephthalic acid to clog the piping during pneumatic transportation. Furthermore, even if inert gas is constantly blown in to fluidize the terephthalic acid in a container storing terephthalic acid, inert gas containing acetic acid will blow up from the outlet at the bottom of the container. As a result, the powdered terephthalic acid at the bottom of the container becomes wet and falls poorly, making it necessary to dismantle and clean the container outlet. Drainage containing condensed acetic acid was collected from the piping, mixed with approximately 100 ppm (weight ratio) of terephthalic acid, esterified with ethylene glycol, and subjected to a polycondensation reaction, resulting in an abnormal color tone in the resulting polyethylene terephthalate. Therefore, it is assumed that the impurities in terephthalic acid concentrate in the drain where acetic acid is condensed, and that these impurities are partially mixed into the terephthalic acid during pneumatic transport, causing a decrease in the quality of the polymer, especially uneven color tone of the polymer. be done.
本発明はこれらの問題を解決し、酢酸を含有す
るテレフタル酸の気力輸送を長期安定に連続して
行うことを可能にし、かつそれを原料とするポリ
エステルの品質低下を防止する方法を提供するも
のであり、酢酸を含有するテレフタル酸を容器か
ら容器へ不活性ガスを循環使用しつつ連続的に気
力輸送するに際し、不活性ガスの循環路に酢酸捕
集装置を設けて、循環再使用する不活性ガス中の
酢酸濃度を、酢酸が凝縮してドレンとなるのを防
止し得る濃度に保持することを特徴とするもので
ある。 The present invention solves these problems and provides a method that enables continuous pneumatic transportation of terephthalic acid containing acetic acid in a stable manner over a long period of time, and prevents deterioration in the quality of polyester made from the same as a raw material. When terephthalic acid containing acetic acid is continuously pneumatically transported from container to container while circulating an inert gas, an acetic acid collection device is installed in the inert gas circulation path, and the inert gas is recycled and reused. It is characterized in that the concentration of acetic acid in the active gas is maintained at a concentration that can prevent acetic acid from condensing and becoming drain.
不活性ガス中の酢酸濃度を、酢酸が凝縮してド
レンとなるのを防止し得る低い濃度に保持するに
は、不活性ガスの循環路に酢酸捕集装置を設ける
ことが必要である。循環再使用する不活性ガスの
一部を大気中に排出して、新しい不活性ガスを捕
充することによつて酢酸濃度を低く保持すること
も可能であるが、経済的見地および公害発生の見
地から好ましくない。 In order to maintain the acetic acid concentration in the inert gas at a low concentration that can prevent acetic acid from condensing and becoming drain, it is necessary to provide an acetic acid collector in the inert gas circulation path. It is possible to keep the acetic acid concentration low by discharging a portion of the recycled inert gas into the atmosphere and capturing new inert gas, but this is not possible from an economic standpoint and due to the risk of pollution. I don't like it from my point of view.
またテレフタル酸の貯蔵容器からのテレフタル
酸の吐出を円滑にするために、不活性ガスを間欠
的に吹き込んでテレフタル酸を流動化させること
が望ましいが、この流動化のための不活性ガスと
しては気力輸送系の循環再使用不活性ガスの一部
を用いてもよいし、新しい不活性ガスを用いて気
力輸送系から洩れる不活性ガスの補充としてもよ
い。 In addition, in order to smoothly discharge terephthalic acid from the terephthalic acid storage container, it is desirable to fluidize the terephthalic acid by intermittently blowing an inert gas into it. A part of the recycled inert gas of the pneumatic transport system may be used, or new inert gas may be used to replenish the inert gas leaking from the pneumatic transport system.
第１図は窒素中での酢酸の飽和濃度と温度の関
係を示す。不活性ガスとして窒素ガスを用いて気
力輸送する場合、輸送系の最低温度に応じて酢酸
濃度をこの曲線より下の範囲に保持すればよい。
（輸送系から除去する酢酸の程度を季節によつて
変えるようにしてもよい。）
第２図は本発明の実施態様の一例を示す概略図
で、テレフタル酸を容器Ａから容器Ｂへ輸送する
気力輸送系を示している。容器Ａよりロータリバ
ルブ１により吐出されたテレフタル酸は不活性ガ
ス配管２より導入された不活性ガスと混合され輸
送配管３によりサイクロン４に入り、ここでテレ
フタル酸は不活性ガスと分離されて容器Ｂ内に供
給される。一方不活性ガスは配管５を経てブロワ
ー６に循環される、配管７は不活性ガスの補給管
で系外に少量洩れる一部のガス量をこれにより補
給する場合に使用する。 FIG. 1 shows the relationship between the saturation concentration of acetic acid in nitrogen and temperature. When carrying out pneumatic transport using nitrogen gas as an inert gas, the acetic acid concentration may be maintained in a range below this curve depending on the lowest temperature of the transport system.
(The degree of acetic acid removed from the transport system may be varied depending on the season.) FIG. 2 is a schematic diagram showing an example of an embodiment of the present invention, in which terephthalic acid is transported from container A to container B. Showing the pneumatic transport system. Terephthalic acid discharged from container A by rotary valve 1 is mixed with inert gas introduced from inert gas pipe 2 and enters cyclone 4 via transport pipe 3, where the terephthalic acid is separated from the inert gas and returned to container. Supplied within B. On the other hand, the inert gas is circulated through the pipe 5 to the blower 6. The pipe 7 is an inert gas replenishment pipe and is used to replenish a small amount of gas that leaks out of the system.
８は循環不活性ガス中の酢酸を捕集する装置で
あり、捕集装置としては、たとえば次のようなも
のが挙げられる。 8 is a device for collecting acetic acid in the circulating inert gas, and examples of the collecting device include the following.
(1) 活性炭、シリカゲル等の吸着剤を使用する吸
着装置
(2) アルカリと接触させて中和除去する接触装置
(3) 酢酸の露点以下にして酢酸を凝縮除去する熱
交換装置
(4) 水および／またはグリコール類などと接触さ
せて吸収除去する気液接触装置
酢酸捕集装置はブロワーの吸込側、吐出側いず
れの位置に取付けてもよいことは言うまでもな
い。不活性ガス中の酢酸濃度は酢酸捕集装置出口
の配管に設置したサンプリング孔９から不活性ガ
スをサンプリングし、ガスクロマトグラフ法にて
測定し、不活性ガス温度はサンプリング孔近辺の
循環不活性ガス配管に設置した温度計１０で測定
するようになつている。(1) Adsorption equipment that uses adsorbents such as activated carbon and silica gel (2) Contact equipment that neutralizes and removes acetic acid by contacting it with alkali (3) Heat exchange equipment that condenses and removes acetic acid at a temperature below the dew point of acetic acid (4) Water and/or a gas-liquid contacting device that absorbs and removes glycols by contacting them. It goes without saying that the acetic acid trapping device may be attached to either the suction side or the discharge side of the blower. The concentration of acetic acid in the inert gas is measured by sampling the inert gas from the sampling hole 9 installed in the piping at the outlet of the acetic acid collection device and measuring it by gas chromatography.The inert gas temperature is measured using the circulating inert gas near the sampling hole. The temperature is measured using a thermometer 10 installed in the pipe.
ブロワー６としてはルーツブロワー、ターボブ
ロワー等が採用され、通常輸送圧力は0.4〜0.8
Kg／cm2Ｇの範囲が採用される。 As the blower 6, a Roots blower, turbo blower, etc. are used, and the transport pressure is usually 0.4 to 0.8.
A range of Kg/cm 2 G is adopted.
また容器Ａにはテレフタル酸を流動化させ吐出
を円滑にするため、配管１１より不活性ガスを間
欠的に吹き込むようになつている。不活性ガスの
圧力は1.0〜1.5Kg／cm2Ｇが適当である。 In addition, an inert gas is intermittently blown into the container A through a pipe 11 in order to fluidize the terephthalic acid and make discharge smooth. The appropriate pressure of the inert gas is 1.0 to 1.5 Kg/cm 2 G.
本発明の方法によれば酢酸の凝縮によるドレン
の発生がなく、またテレフタル酸貯蔵容器の吐出
口からの酢酸含有不活性ガスの吹き上がりにより
酢酸が凝縮して容器下部のテレフタル酸が固着し
て吐出不良となることが防止され、酢酸を含有す
るテレフタル酸の気力輸送が長期安定して可能に
なり、さらにテレフタル酸の不純分が集中した酢
酸の凝縮ドレンがテレフタル酸中に混入すること
がなくなり、それを原料とするポリマーの品質低
下が防止される。 According to the method of the present invention, there is no generation of drainage due to condensation of acetic acid, and the acetic acid is condensed due to the blowing up of acetic acid-containing inert gas from the outlet of the terephthalic acid storage container, and the terephthalic acid at the bottom of the container is fixed. This prevents discharge failures, enables stable pneumatic transport of terephthalic acid containing acetic acid over a long period of time, and also prevents acetic acid condensed drain containing concentrated terephthalic acid impurities from mixing into terephthalic acid. This prevents deterioration in the quality of polymers made from it.
以下本発明の実施例を示す。 Examples of the present invention will be shown below.
実施例
第１図に示すように気力輸送系にて酢酸含有量
180ppm（重量比）のテレフタル酸の輸送を行つ
た。Example: As shown in Figure 1, acetic acid content in a pneumatic transport system.
180ppm (by weight) of terephthalic acid was transported.
容器Ａとしては500m2のサイロ、容器Ｂとして
は20m2のサイロ、ブロワー６としてはルーツブロ
ワー、酢酸捕集装置８としては活性炭塔を使用し
た。サイロＡからサイロＢまでの距離は水平距離
で25m、垂直距離で15mであり、輸送配管の内径
は200mmであつた。輸送動力気体として窒素ガス
を使用し、ルーツブロワー出口圧力は0.6Kg／cm2
Ｇ、流量は75m2／minで毎時25トンのテレフタル
酸を輸送した。またサイロＡのテレフタル酸を配
管１１により1.3Kg／cm2Ｇの窒素をつねに１分間
隔で10秒間連続して吹ひ込んでテレフタル酸を流
動化した。系外に洩れる一部の窒素ガスはサイロ
Ａのテレフタル酸の流動化に使用した窒素で補充
できたので配管７による窒素の補給は行わなかつ
た。 A 500 m 2 silo was used as container A, a 20 m 2 silo was used as container B, a Roots blower was used as blower 6, and an activated carbon tower was used as acetic acid collector 8. The distance from Silo A to Silo B was 25 m horizontally and 15 m vertically, and the inner diameter of the transport pipe was 200 mm. Nitrogen gas is used as the transportation power gas, and the Roots blower outlet pressure is 0.6Kg/cm 2
G, the flow rate was 75 m 2 /min, and 25 tons of terephthalic acid was transported per hour. Further, the terephthalic acid in the silo A was fluidized by continuously blowing nitrogen of 1.3 kg/cm 2 G into the silo A at 1 minute intervals for 10 seconds through the pipe 11. Part of the nitrogen gas leaking out of the system could be replenished with the nitrogen used to fluidize the terephthalic acid in silo A, so nitrogen supply through piping 7 was not performed.
テレフタル酸の気力輸送に際しては窒素ガス中
の酢酸を活性炭塔で吸着し窒素中の酢酸濃度を
4000ppm（容量比）以下に保つた。テレフタル
酸の輸送を１日150トンで３ケ月行つたが、輸送
管中には酢酸ドレンはなく、サイロＡからテレフ
タル酸の吐出は良好であり、輸送能力の低下は認
められず、また酢酸ドレンにテレフタル酸の不純
分が集中してこれがテレフタル酸に混入してポリ
マーの品質低下をもたらすこともなかつた。この
期間中の循環再使用する不活性ガスの最低温度は
５℃であつた。 When transporting terephthalic acid pneumatically, acetic acid in nitrogen gas is adsorbed in an activated carbon column to reduce the concentration of acetic acid in nitrogen.
It was kept below 4000ppm (capacity ratio). Terephthalic acid was transported at a rate of 150 tons per day for three months, but there was no acetic acid drain in the transport pipe, terephthalic acid was discharged well from Silo A, and no decrease in transport capacity was observed. Impurities of terephthalic acid were not concentrated in the terephthalic acid and mixed with the terephthalic acid, resulting in no deterioration in the quality of the polymer. The minimum temperature of the recirculated inert gas during this period was 5°C.
第１図は窒素中での酢酸の飽和濃度と温度の関
係を示す図、第２図は本発明の実施態様の一例を
示す概略図でテレフタル酸を容器Ａから容器Ｂへ
輸送する気力輸送系を示し、８は酢酸捕集装置を
示す。
Fig. 1 is a diagram showing the relationship between the saturation concentration of acetic acid in nitrogen and temperature, and Fig. 2 is a schematic diagram showing an example of an embodiment of the present invention, showing a pneumatic transport system for transporting terephthalic acid from container A to container B. 8 indicates an acetic acid collection device.
Claims (1)
へ不活性ガスを循環使用しつつ連続的に気力輸送
するに際し、不活性ガスの循環路に酢酸捕集装置
を設けて、循環再使用する不活性ガス中の酢酸濃
度を、酢酸が擬縮してドレンとなるのを防止し得
る濃度に保持することを特徴とするテレフタル酸
の輸送方法。 ２ 酢酸を含有するテレフタル酸の酢酸量が
20ppm（重量比）以上である特許請求の範囲第
１項記載の方法。[Scope of Claims] 1. When terephthalic acid containing acetic acid is continuously pneumatically transported from container to container while circulating inert gas, an acetic acid collection device is provided in the inert gas circulation path to A method for transporting terephthalic acid, which comprises maintaining the concentration of acetic acid in an inert gas to be reused at a concentration that can prevent acetic acid from pseudo-condensing and becoming drain. 2 The amount of acetic acid in terephthalic acid containing acetic acid is
The method according to claim 1, wherein the content is 20 ppm (weight ratio) or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11756978A JPS5543060A (en) | 1978-09-25 | 1978-09-25 | Transportation of terephthalic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11756978A JPS5543060A (en) | 1978-09-25 | 1978-09-25 | Transportation of terephthalic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5543060A JPS5543060A (en) | 1980-03-26 |
| JPS6132300B2 true JPS6132300B2 (en) | 1986-07-25 |
Family
ID=14715058
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11756978A Granted JPS5543060A (en) | 1978-09-25 | 1978-09-25 | Transportation of terephthalic acid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5543060A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006321997A (en) * | 2005-04-22 | 2006-11-30 | Mitsubishi Chemicals Corp | Method for producing polyester |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5102632A (en) * | 1990-12-21 | 1992-04-07 | Metallgesellschaft Aktiengesellschaft | Two-step method for recovering dispersed noble metals |
| JP2006321996A (en) * | 2005-04-22 | 2006-11-30 | Mitsubishi Chemicals Corp | Method for producing polyester |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS516935A (en) * | 1974-07-05 | 1976-01-20 | Mitsubishi Chem Ind | Terefutarusanno isohoho |
-
1978
- 1978-09-25 JP JP11756978A patent/JPS5543060A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS516935A (en) * | 1974-07-05 | 1976-01-20 | Mitsubishi Chem Ind | Terefutarusanno isohoho |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006321997A (en) * | 2005-04-22 | 2006-11-30 | Mitsubishi Chemicals Corp | Method for producing polyester |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5543060A (en) | 1980-03-26 |
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