JPS6138124B2 - - Google Patents
Info
- Publication number
- JPS6138124B2 JPS6138124B2 JP53107077A JP10707778A JPS6138124B2 JP S6138124 B2 JPS6138124 B2 JP S6138124B2 JP 53107077 A JP53107077 A JP 53107077A JP 10707778 A JP10707778 A JP 10707778A JP S6138124 B2 JPS6138124 B2 JP S6138124B2
- Authority
- JP
- Japan
- Prior art keywords
- organic solvent
- carbon dioxide
- carbonic acid
- methanol
- present
- 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
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 61
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 51
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 21
- 239000001569 carbon dioxide Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 15
- 239000003960 organic solvent Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000005194 fractionation Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 description 9
- 238000001816 cooling Methods 0.000 description 5
- 230000008014 freezing Effects 0.000 description 5
- 238000007710 freezing Methods 0.000 description 5
- 235000011089 carbon dioxide Nutrition 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000003507 refrigerant Substances 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 235000014214 soft drink Nutrition 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Description
【発明の詳細な説明】
本発明は液化炭酸の製造方法に関するものであ
り、更に詳しく述べれば、冷源としてL.N.G.を
利用して冷却した低温の親水性の有機溶媒を使用
して安価に液化炭酸を製造する方法に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing liquefied carbonic acid, and more specifically, the present invention relates to a method for producing liquefied carbonic acid. The present invention relates to a method for manufacturing.
液化炭酸は、食品冷凍冷却用、清涼飲料水、消
火器、鋳物用鋳型硬化剤、化学工業用などの広い
方面にわたつて利用されている有用な工業薬品で
ある。 Liquefied carbonic acid is a useful industrial chemical that is used in a wide range of applications, including food freezing and cooling, soft drinks, fire extinguishers, mold hardening agents for foundries, and chemical industry applications.
従来液化炭酸を製造するには精製した炭酸ガス
を10〜20Kg／cm2に圧縮しこれを−20〜−40℃に冷
却して製造していた。この際本発明に利用するご
とく、L.N.G.を気化する際の潜熱を冷却に利用
すれば、従来のアンモニア又はフロンガス等の冷
凍サイクルに比べて安価に製造することが出来る
のは当然であるが、炭酸ガスを圧縮するための動
力費が未だ高価につく。そこで本出願人はさきに
特願昭52―3168号（特開昭53―88692号）におい
て圧縮機による圧縮工程を必要としない液化炭酸
の製造装置を出願した。 Conventionally, liquefied carbonic acid was produced by compressing purified carbon dioxide gas to 10 to 20 kg/cm 2 and cooling it to -20 to -40°C. In this case, if the latent heat during vaporization of LNG is used for cooling as in the present invention, it is natural that it can be produced at a lower cost compared to conventional refrigeration cycles such as ammonia or fluorocarbon gas, but carbon dioxide Power costs for compressing gas are still high. Therefore, the present applicant previously filed an application in Japanese Patent Application No. 52-3168 (Japanese Unexamined Patent Publication No. 53-88692) for an apparatus for producing liquefied carbonic acid that does not require a compression process using a compressor.
しかしながら前者に於ては容量の大きい圧縮機
を要し機械エネルギーの消費が大であるため未だ
コスト高となり、後者に於ては装置がかなり大き
くなると共に、加熱エネルギー、冷熱共に無駄に
使用される面が多く完全な方法とは言えなかつ
た。 However, the former requires a large-capacity compressor and consumes a large amount of mechanical energy, so it is still costly, while the latter requires a considerably larger device and wastes both heating energy and cooling energy. There were many aspects to this method, and it could not be called a perfect method.
また特公昭52―28752号公報に記載の溶媒とし
て低温のトリクレンを使用する方法があるが、こ
の方法は解氷のため装置を切換える必要のあるこ
と、少量でもドライアイスを生じると溶媒の性質
上好ましくないので厳密な温度、圧力のコントロ
ールを必要とし操作が煩雑であること、液化炭酸
中に溶媒混入のおそれのあるプロセスであるため
毒性の問題を生じる可能性のあること等種々の欠
点を有している。 In addition, there is a method using low-temperature trichlene as a solvent as described in Japanese Patent Publication No. 52-28752, but this method requires changing the equipment to melt the ice, and due to the nature of the solvent, even a small amount of dry ice may be generated. This process is undesirable and requires strict temperature and pressure control, making the operation complicated, and the process may cause toxicity problems due to the possibility of solvent being mixed into the liquefied carbonic acid. are doing.
本発明者等はこのような状況に鑑み、極めて安
価な液化炭酸の製造方法について検討を重ねた結
果親水性の有機溶媒を利用することに想到し本発
明に到つた。 In view of this situation, the inventors of the present invention have repeatedly studied methods for producing liquefied carbonic acid at extremely low cost, and as a result, they have come up with the idea of using a hydrophilic organic solvent and have arrived at the present invention.
即ち本発明の目的は、冷却エネルギーとしてL.
N.G.のような特に低温で安価な冷凍を使用しま
た機械的エネルギーとして圧縮機によらずポンプ
のみを使用し、従来の方法に比べ大巾に安価な液
化炭酸を製造する方法を提供するにある。 That is, the purpose of the present invention is to use L. as cooling energy.
To provide a method for producing liquefied carbon dioxide that is significantly cheaper than conventional methods by using particularly low-temperature and inexpensive refrigeration such as NG and by using only a pump instead of a compressor for mechanical energy. .
而して本発明の要旨は原料炭酸ガスを三重点未
満の圧力で低温の有機溶媒に吸収しこの有機溶媒
中に凝縮せしめ、この液を三重点以上の加圧分留
塔に圧送して分留すること。並びに、前記有機溶
媒の一部を分流し精留により水を系外に分離する
ことを特徴とする液化炭酸の製造方法である。前
記吸収に際しては低温のため若干のドライアイス
が生成し、これが液中に浮遊する状態となつても
さしつかえない。 The gist of the present invention is to absorb carbon dioxide as a raw material into a low-temperature organic solvent at a pressure below the triple point, condense it in this organic solvent, and separate the liquid by pumping it to a pressure fractionation column at a pressure above the triple point. to stay. Furthermore, the method for producing liquefied carbonic acid is characterized in that part of the organic solvent is diverted and water is separated from the system by rectification. During the absorption, some dry ice is generated due to the low temperature, and there is no problem even if this becomes suspended in the liquid.
具体例について述べれば、原料炭酸ガスを冷却
器を備えた吸収塔内に導入して三重点未満の圧力
（通常は原料炭酸ガスのまま）でL.N.G.の気化潜
熱を利用して−70〜−80℃以下に冷却したメタノ
ールと向流接触させ炭酸ガスをメタノールに吸収
させる。この際若干量のドライアイスが生成して
もさしつかえない。この吸収液を加圧分留塔に圧
送し三重点以上の圧力下で、０〜10℃付近の温度
に加熱してメタノールと炭酸ガスに分離精製し、
再生したメタノールを再び吸収塔へ循環使用する
ことにより液化炭酸を連続的に製造するものであ
る。 To give a concrete example, feedstock carbon dioxide gas is introduced into an absorption tower equipped with a cooler, and the latent heat of vaporization of LNG is used at a pressure below the triple point (normally the feedstock carbon dioxide remains) to -70 to -80 It is brought into countercurrent contact with methanol cooled to below ℃ to absorb carbon dioxide gas into methanol. At this time, it is acceptable even if a small amount of dry ice is generated. This absorption liquid is sent under pressure to a pressure fractionation column and heated to a temperature around 0 to 10°C under pressure above the triple point to separate and purify it into methanol and carbon dioxide gas,
Liquefied carbonic acid is continuously produced by recycling the regenerated methanol to the absorption tower.
なお原料炭酸ガスと同伴する水分はメタノール
に吸収されるが、加圧分留塔からの再生メタノー
ルの一部を分流し精留することにより此の水分は
系外に取り出される。 Note that the water accompanying the raw carbon dioxide gas is absorbed by methanol, but this water is taken out of the system by diverting and rectifying a part of the regenerated methanol from the pressure fractionator.
従つて原料ガスは氷結を生じる手前の温度まで
予冷してドレンを切つておくのみでよく従来のよ
うに氷結解氷をくりかえし行なう煩雑な脱水工程
を省略することができ、これも本発明の工業的に
すぐれた点である。 Therefore, the raw material gas only needs to be pre-cooled to a temperature just before freezing and the drain is cut off, and the complicated dehydration process of repeatedly freezing and thawing as in the past can be omitted, which is also an advantage of the present invention. This is an excellent point.
本発明で用いる有機溶媒としては、低級脂肪
酸、低級アルコール、エステル等水溶性であつて
融点が−70〜−80℃以下のものであればいずれも
使用できるが、入手しやすいメタノール、エタノ
ール、アセトン、酢酸エチル等を使用すれば工業
的に有利である。特に製品の毒性が問題となるよ
うな食品に関する用途の場合にはエタノールの如
き無害の溶媒を使用することにより、そのような
懸念を全く解消できることも本発明のすぐれた点
である。 As the organic solvent used in the present invention, any water-soluble organic solvent such as lower fatty acids, lower alcohols, and esters with a melting point of -70 to -80°C or lower can be used, but readily available methanol, ethanol, acetone, etc. , ethyl acetate, etc. are industrially advantageous. Particularly in the case of food-related applications where the toxicity of the product is a problem, it is an advantage of the present invention that such concerns can be completely eliminated by using a harmless solvent such as ethanol.
次に本発明の方法を工業的に実施する場合の一
例を図面について説明する。 Next, an example of industrial implementation of the method of the present invention will be described with reference to the drawings.
露点２℃CO298％を含む原料炭酸ガスは、L.N.
G.による冷却器１を備え、良好な気液接触を行
なうことが出来る充てん塔２に入り、ガスは上昇
しながら上から流下する−80℃に冷却されたメタ
ノールと向流接触する。炭酸ガスを吸収したメタ
ノールはポンプ３で三重点以上の圧力例えば６
Kg／cm2Ｇに加圧され、次いで熱交換器４で加圧分
留塔５を出た再生メタノールと熱交換することに
より予熱され、底部に加熱装置６を備えた加圧分
留塔５の中段に送入される。加圧分留塔５は吸収
塔２と同様に例えば充てん塔よりなり、ここで例
えば６Kg／cm2Ｇに加圧、５℃に加熱して炭酸ガス
の精留とメタノールの再生を行なう。此の温度レ
ベルが低く選定できるので、水、大気等の保有熱
量を熱源とすることが出来る。加圧分留塔５を出
た炭酸ガスは凝縮器７においてL.N.G.などの冷
媒により冷却して液化される。炭酸ガスの吸収と
同時にメタノールに溶解した不純ガスは還流冷却
器８で分離して形外へ放出される。一方液化した
炭酸ガス（液化炭酸）はその一部を製品として抜
出し液化炭酸貯槽９に送られ、他は再び加圧分留
塔５に還流して炭酸ガスの精留を行なう。 The raw carbon dioxide gas containing 98% CO2 with a dew point of 2℃ is LN.
The gas enters a packed tower 2 equipped with a cooler 1 according to G. G. and capable of good gas-liquid contact, and as the gas rises, it comes into countercurrent contact with methanol cooled to -80°C flowing down from above. Methanol that has absorbed carbon dioxide gas is pumped to pump 3 where it is pumped to a pressure above the triple point, e.g. 6
The pressurized fractionator 5 is pressurized to Kg/cm 2 G, then preheated by exchanging heat with the regenerated methanol exiting the pressure fractionator 5 in the heat exchanger 4, and equipped with a heating device 6 at the bottom. It is sent to the middle row of. Like the absorption tower 2, the pressure fractionating tower 5 is, for example, a packed tower, and is pressurized to, for example, 6 kg/cm 2 G and heated to 5° C. to rectify carbon dioxide gas and regenerate methanol. Since this temperature level can be selected to be low, the amount of heat held by water, the atmosphere, etc. can be used as the heat source. The carbon dioxide gas exiting the pressurized fractionator 5 is cooled and liquefied by a refrigerant such as LNG in a condenser 7. Simultaneously with absorption of carbon dioxide gas, impurity gas dissolved in methanol is separated in a reflux condenser 8 and discharged outside the mold. On the other hand, a part of the liquefied carbon dioxide (liquefied carbonic acid) is extracted as a product and sent to the liquefied carbonic acid storage tank 9, and the other part is refluxed to the pressurized fractionator 5 again for rectification of carbon dioxide gas.
再生されたメタノールは加圧分留塔５の底部よ
り抜き出され、炭酸ガスを吸収したメタノールと
の熱交換器４およびL.N.G.のごとき冷媒が循環
している冷却器１３を経て吸収塔２の操業温度−
70℃ないし−80℃に冷却され、再び吸収塔２に戻
されるが、その間に一部分流され底部に加熱装置
１０を備えた精留塔１１の中段へ送入される。精
留塔１１は例えば棚段塔よりなりここで加熱装置
１０で加熱してメタノールと水との分離精製を行
なう。精留塔１１の上部より出たメタノールは凝
縮器において冷却して液化される。その一部は冷
却器１３を経て再び吸収塔２に戻されるが、他は
再び精留塔１１に還流される。 Regenerated methanol is extracted from the bottom of the pressurized fractionator 5, passes through a heat exchanger 4 with methanol that has absorbed carbon dioxide gas, and a cooler 13 in which a refrigerant such as LNG is circulated, and is then used to operate the absorption tower 2. Temperature -
It is cooled to 70 DEG C. to -80 DEG C. and returned to the absorption tower 2, during which time it is partially washed away and sent to the middle stage of a rectification tower 11 equipped with a heating device 10 at the bottom. The rectifying column 11 is composed of, for example, a tray column, and is heated by a heating device 10 to separate and purify methanol and water. Methanol discharged from the upper part of the rectification column 11 is cooled and liquefied in a condenser. A part of it is returned to the absorption tower 2 via the cooler 13, while the rest is refluxed to the rectification tower 11 again.
実施の一例として0.2Kg／cm2Ｇの原料炭酸ガス
を使用した場合、本発明によると液化炭酸1Tを
製造するに要した電力は約7KWHであつた。（従
来法の場合、電力は70〜150KWHが普通であ
る。）
本発明の実施により液化炭酸を製造する場合に
は、次のような効果がある。 As an example of implementation, when 0.2 Kg/cm 2 G of raw carbon dioxide gas was used, the electric power required to produce 1 T of liquefied carbonic acid according to the present invention was about 7 KWH. (In the case of the conventional method, the electric power is usually 70 to 150 KWH.) When liquefied carbonic acid is produced by implementing the present invention, the following effects are obtained.
(1) 液化炭酸は食品冷凍用、清涼飲料水等の食品
関係に使用されており、前記特公昭52―28752
号記載の発明におけるごとくトリクレンを使用
した場合には毒性の問題があるが、本発明に於
てはこれを簡単に回避することができる。（例
えばエタノール使用）
(2) 非親水性の例えばトリクレンを溶媒として使
用した場合系内で氷結が起り、装置の切り換え
により解氷して氷を系外に取出す必要がある
が、本発明の場合には溶媒の一部を抜出し精留
することにより連続的に水を分離することがで
きるので安定な運転を行ない易い。(1) Liquefied carbonic acid is used for food products such as food freezing and soft drinks.
Although there is a problem of toxicity when triclene is used as in the invention described in the above, this problem can be easily avoided in the present invention. (For example, using ethanol) (2) If a non-hydrophilic solvent such as trichlene is used as a solvent, freezing will occur in the system, and it is necessary to change the equipment to thaw the ice and take the ice out of the system, but in the case of the present invention Since water can be continuously separated by extracting a portion of the solvent and rectifying it, stable operation is easy.
第１図は本発明方法のフローシートである。 FIG. 1 is a flow sheet of the method of the present invention.
Claims (1)
親水性有機溶媒に吸収しあるいはさらに該有機溶
媒中に一部凝結固体炭酸として含有せしめ、この
液を三重点以上の加圧分留塔に圧送し分留するこ
とを特徴とする液化炭酸の製造方法。 ２ 親水性有機溶媒の一部を分流し、精留により
水を分離し溶媒を循環する工程を設けた特許請求
の範囲１記載の方法。 ３ 前記有機溶媒がメタノールである特許請求の
範囲１記載の方法。 ４ 前記有機溶媒がエタノールである特許請求の
範囲１記載の方法。 ５ 前記有機溶媒を低温にするための冷源として
L.N.Gを使用する特許請求の範囲１記載の方法。[Claims] 1. Carbon dioxide as a raw material is absorbed into a low-temperature hydrophilic organic solvent at a pressure below the triple point, or is further contained in the organic solvent as a partially condensed solid carbon dioxide. A method for producing liquefied carbonic acid, which comprises feeding the carbonic acid under pressure to a pressurized fractionation column and fractionating it. 2. The method according to claim 1, further comprising a step of separating a portion of the hydrophilic organic solvent, separating water by rectification, and circulating the solvent. 3. The method according to claim 1, wherein the organic solvent is methanol. 4. The method according to claim 1, wherein the organic solvent is ethanol. 5. As a cold source to bring the organic solvent to a low temperature
The method according to claim 1 using LNG.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10707778A JPS5532784A (en) | 1978-08-31 | 1978-08-31 | Production of liquefied carbon dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10707778A JPS5532784A (en) | 1978-08-31 | 1978-08-31 | Production of liquefied carbon dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5532784A JPS5532784A (en) | 1980-03-07 |
| JPS6138124B2 true JPS6138124B2 (en) | 1986-08-27 |
Family
ID=14449889
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10707778A Granted JPS5532784A (en) | 1978-08-31 | 1978-08-31 | Production of liquefied carbon dioxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5532784A (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4960340A (en) * | 1987-01-23 | 1990-10-02 | Kabushiki Kaisha Sakurakurepasu | Implement for applying liquid |
| US4867593A (en) * | 1987-01-30 | 1989-09-19 | Pentel Kabushiki Kaisha | Liquid dispenser with valve mechanism and flexible container |
| US4966483A (en) * | 1987-11-12 | 1990-10-30 | Ancos Co., Ltd. | Valve operating mechanism |
| FR2954179B1 (en) * | 2009-12-22 | 2014-03-28 | Air Liquide | METHOD AND APPARATUS FOR DRYING AND COMPRESSING A CO2-RICH FLOW |
| CN113959178B (en) * | 2021-11-29 | 2023-01-20 | 李欣锐 | Carbon capture method in hydrogen production process by LNG |
-
1978
- 1978-08-31 JP JP10707778A patent/JPS5532784A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5532784A (en) | 1980-03-07 |
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