JPH0629129B2 - Method for producing phosgene - Google Patents
Method for producing phosgeneInfo
- Publication number
- JPH0629129B2 JPH0629129B2 JP63156040A JP15604088A JPH0629129B2 JP H0629129 B2 JPH0629129 B2 JP H0629129B2 JP 63156040 A JP63156040 A JP 63156040A JP 15604088 A JP15604088 A JP 15604088A JP H0629129 B2 JPH0629129 B2 JP H0629129B2
- Authority
- JP
- Japan
- Prior art keywords
- phosgene
- activated carbon
- reaction
- catalyst
- carbon
- 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 - Lifetime
Links
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 title claims description 29
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 63
- 239000003054 catalyst Substances 0.000 claims description 19
- 229910052751 metal Inorganic materials 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 18
- 239000000460 chlorine Substances 0.000 claims description 10
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 9
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 9
- 229910052801 chlorine Inorganic materials 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 229910052723 transition metal Inorganic materials 0.000 claims description 4
- 150000003624 transition metals Chemical class 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 30
- 238000000034 method Methods 0.000 description 13
- 239000006227 byproduct Substances 0.000 description 9
- 239000010410 layer Substances 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000002994 raw material Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000008346 aqueous phase Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 229920000515 polycarbonate Polymers 0.000 description 4
- 239000004417 polycarbonate Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 235000013162 Cocos nucifera Nutrition 0.000 description 3
- 244000060011 Cocos nucifera Species 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 3
- 150000001342 alkaline earth metals Chemical class 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- GCXUHGZBBGZTII-UHFFFAOYSA-N a828071 Chemical compound ClC(Cl)=O.ClC(Cl)=O GCXUHGZBBGZTII-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000003077 lignite Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003415 peat Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はホスゲンの製造方法に関し、詳しくは特定の触
媒を使用することによって、一酸化炭素と塩素とから高
純度のホスゲンを効率よく製造する方法に関する。TECHNICAL FIELD The present invention relates to a method for producing phosgene, and more specifically, it efficiently produces high-purity phosgene from carbon monoxide and chlorine by using a specific catalyst. Regarding the method.
従来から、一酸化炭素と塩素とを反応させてホスゲンを
製造するにあたって、活性炭を触媒として用いることが
知られている。しかし、活性炭をそのまま触媒として用
いた場合には、得られるホスゲンは多量の不純物、特に
四塩化炭素を含有するものとなる。このように多量の四
塩化炭素を含有するホスゲンを原料として、ポリカーボ
ネートを製造すると、その四塩化炭素の影響で得られる
ポリカーボネートの品質が低下するという問題がある。
したがって、ホスゲン中に含まれる四塩化炭素等の不純
物をできるだけ少なくすることが、高品質のポリカーボ
ネートを製造する上で望まれている。It has been conventionally known to use activated carbon as a catalyst when phosgene is produced by reacting carbon monoxide with chlorine. However, when activated carbon is used as it is as a catalyst, the obtained phosgene contains a large amount of impurities, especially carbon tetrachloride. When a polycarbonate is produced by using phosgene containing a large amount of carbon tetrachloride as a raw material, there is a problem that the quality of the obtained polycarbonate deteriorates due to the influence of the carbon tetrachloride.
Therefore, it is desired to reduce impurities such as carbon tetrachloride contained in phosgene as much as possible in order to produce high quality polycarbonate.
ところで、一般に触媒を用いる反応では、それが発熱反
応であれば、その熱により触媒層の中央部が特に加熱さ
れることが知られている。このことはホスゲンの製造に
関しても同様であり、一酸化炭素と塩素との反応により
触媒層の中央部が加熱され、外部冷却により触媒層出口
温度を７０〜９０℃程度に下げても、触媒層の一部は４
５０℃以上もの高温になる。そのため、ホスゲンの製造
時に副生成物である四塩化炭素が多量に生成するという
問題がある（Kirk-Othmer,“Encyclopedia of Chemical
Technology”，第２版，第５巻）。しかも、加熱され
た触媒層の部分を、外部冷却や反応ガスの希釈等によっ
て所定温度以下に冷却することは極めて困難である。By the way, in a reaction using a catalyst, it is generally known that if the reaction is an exothermic reaction, the heat particularly heats the central portion of the catalyst layer. This also applies to the production of phosgene. Even if the catalyst layer outlet temperature is lowered to about 70 to 90 ° C. by external cooling, the central portion of the catalyst layer is heated by the reaction of carbon monoxide and chlorine, and Part of is 4
It reaches temperatures as high as 50 ° C or higher. Therefore, there is a problem that a large amount of carbon tetrachloride, which is a by-product, is produced during the production of phosgene (Kirk-Othmer, “Encyclopedia of Chemical
Technology ", Second Edition, Volume 5). Moreover, it is extremely difficult to cool the heated catalyst layer portion to a predetermined temperature or lower by external cooling, dilution of the reaction gas, or the like.
このような副生物の生成を抑制する方法として、反応原
料ガスを触媒層を通過させることなく、触媒充填層面に
接触させ、該触媒充填層の表層部で反応させる装置を用
いてホスゲンを製造する方法が開発されている（特公昭
５５−１４０４４号公報）。しかしながら、この方法に
よっても、四塩化炭素の副生を充分に低減することはで
きない。As a method for suppressing the formation of such by-products, phosgene is produced using a device in which a reaction raw material gas is brought into contact with the surface of a catalyst-packed layer without passing through the catalyst layer and reacted at the surface layer of the catalyst-packed layer. A method has been developed (Japanese Patent Publication No. 55-14044). However, even this method cannot sufficiently reduce the by-product of carbon tetrachloride.
そこで、本発明者らは上記従来技術の課題を解決し、副
生物の少ない高純度のホスゲンを効率よく製造する方法
を開発すべく鋭意研究を重ねた。Therefore, the inventors of the present invention have conducted earnest studies to solve the above-mentioned problems of the prior art and to develop a method for efficiently producing high-purity phosgene with less by-products.
その結果、触媒として用いる活性炭中の金属分含量を酸
洗浄により1.5重量％以下に低減することにより、上記
課題を解決できることを見出した。本発明はかかる知見
に基いて完成したものである。As a result, they have found that the above problem can be solved by reducing the metal content in activated carbon used as a catalyst to 1.5% by weight or less by acid washing. The present invention has been completed based on such findings.
すなわち、本発明は活性炭を触媒とし、一酸化炭素と塩
素とを反応させてホスゲンを製造する方法において、活
性炭を酸洗浄して得られる、遷移金属、ホウ素、アルミ
ニウム又は珪素からなる金属成分の合計が1.5重量％以
下の活性炭を使用することを特徴とするホスゲンの製造
方法を提供するものである。That is, the present invention is a method of producing phosgene by reacting carbon monoxide and chlorine with activated carbon as a catalyst, obtained by acid-washing activated carbon, the total of metal components consisting of transition metal, boron, aluminum or silicon. The present invention provides a method for producing phosgene, which comprises using 1.5% by weight or less of activated carbon.
本発明の方法における一酸化炭素と塩素との反応は、 ＣＯ＋Ｃｌ２→ＣＯＣｌ２ なる反応式にしたがって進行するものである。この反応
は公知の反応であり、原料である一酸化炭素，塩素の割
合や反応条件（温度，圧力等）は、特に制限はなく公知
の方法に準ずればよい。The reaction between carbon monoxide and chlorine in the method of the present invention proceeds according to the reaction formula CO + Cl 2 → COCl 2 . This reaction is a known reaction, and the ratio of the raw materials carbon monoxide and chlorine and the reaction conditions (temperature, pressure, etc.) are not particularly limited and may be in accordance with a known method.
本発明の方法では、上記の反応を活性炭触媒の存在下で
進行させるが、この活性炭中の特定の金属分含量を酸洗
浄により1.5重量％以下、好ましくは1.0重量％以下に調
節する。ここで特定の金属分含量が1.5重量％を超える
ものでは、副生成物である四塩化炭素の生成量を抑制す
ることができない。なお、含量を制御すべき特定の金属
の種類は、Ｔｉ，Ｚｒ，Ｖ，Ｃｒ，Ｍｏ，Ｗ，Ｍｎ，Ｆ
ｅ，Ｃｏ，Ｎｉ等の遷移金属，Ｂ，Ａｌ及びＳｉであ
る。Ｎａ，Ｋ，Ｍｇ，Ｃａ等のアルカリ金属やアルカリ
土類金属は副生成物の生成に影響がほとんどないので、
これらの金属については、前記金属分含量の計算から除
外することができる。つまり、このアルカリ金属やアル
カリ土類金属の含有量は、少なければ問題はないが、た
とえ1.5重量％を超える場合（アルカリ金属やアルカリ
土類金属の量として、あるいはアルカリ金属やアルカリ
土類金属と前記遷移金属等の合計量として）であって
も、副生成物の生成を抑制することは可能であり、本発
明の目的を達成する上で支障となることはない。In the method of the present invention, the above reaction is allowed to proceed in the presence of an activated carbon catalyst, but the specific metal content in this activated carbon is adjusted to 1.5% by weight or less, preferably 1.0% by weight or less by acid washing. Here, if the specific metal content exceeds 1.5% by weight, the amount of carbon tetrachloride as a by-product cannot be suppressed. The specific metal types whose contents should be controlled are Ti, Zr, V, Cr, Mo, W, Mn and F.
e, Co, Ni and other transition metals, B, Al and Si. Alkali metals and alkaline earth metals such as Na, K, Mg and Ca have almost no effect on the production of by-products,
These metals can be excluded from the calculation of the metal content. In other words, if the content of this alkali metal or alkaline earth metal is small, there is no problem, but even if it exceeds 1.5% by weight (as the amount of alkali metal or alkaline earth metal, or Even if it is the total amount of the transition metal), it is possible to suppress the production of by-products and does not hinder the achievement of the object of the present invention.
また、ここで用いる活性炭としては、粉末活性炭，造粒
活性炭など様々であり、特に制限はない。さらに原料の
種類も、木材，ノコギリクズ，ヤシの実の殻，リグニ
ン，亜炭，褐炭，泥炭，石炭など各種のものが使用可能
であり、その調製法についても水蒸気賦活法，薬品賦活
法，その他の各種方法によればよい。Further, the activated carbon used here includes various types such as powdered activated carbon and granulated activated carbon, and is not particularly limited. Furthermore, various kinds of raw materials such as wood, sawdust, coconut shell, lignin, lignite, lignite, peat, coal can be used. Various methods may be used.
本発明の金属分含量1.5重量％以下の活性炭を得るにあ
たっては、上述の活性炭（これは通常２重量％以上の金
属分を含有している。）を、各種方法により酸洗浄しな
ければならない。有効な具体的洗浄方法としては、塩
酸，硫酸，硝酸等の酸で酸洗浄することにより金属分を
除去し、次いで洗浄水にて水相が中性になるまで充分に
洗浄し、しかる後に乾燥する方法があげられる。In order to obtain the activated carbon having a metal content of 1.5% by weight or less of the present invention, the above-mentioned activated carbon (which usually contains 2% by weight or more of a metal) must be acid-washed by various methods. An effective concrete washing method is to remove the metal content by acid washing with an acid such as hydrochloric acid, sulfuric acid, nitric acid, and then wash thoroughly with washing water until the aqueous phase becomes neutral, and then dry. There is a way to do it.
このようにして得られる金属分含量の少ない活性炭を触
媒として用い、以下常法にしたがって一酸化炭素と塩素
とを反応させれば、四塩化炭素等の副生成物の極めて少
ない高純度のホスゲンを製造することができる。By using activated carbon having a low metal content thus obtained as a catalyst and reacting carbon monoxide with chlorine according to a conventional method, highly purified phosgene having a very small amount of by-products such as carbon tetrachloride can be obtained. It can be manufactured.
次に、本発明を実施例および比較例に基いてさらに詳し
く説明する。Next, the present invention will be described in more detail based on Examples and Comparative Examples.
実施例１ （１）触媒の調製 市販の粒状活性炭Ａ（直径1.2〜2.4mmに粉砕したヤシ殻
炭；Ｓｉ1.07wt％，Ａｌ0.9wt％，Ｆｅ0.36wt％，その
他0.012wt％（合計金属分含量2.33wt％））を、１５℃
で濃度１０％の塩酸に投入し、２時間攪拌洗浄後、水相
が中性になるまで充分に水洗し、真空乾燥して、活性炭
Ｃ（Ｓｉ0.46wt％，Ａｌ0.1wt％，Ｆｅ0.01wt％，その
他0.001wt％（合計金属分含量0.57wt％））を得た。Example 1 (1) Preparation of catalyst Commercially available granular activated carbon A (coconut shell coal pulverized to a diameter of 1.2 to 2.4 mm; Si 1.07 wt%, Al 0.9 wt%, Fe 0.36 wt%, other 0.012 wt% (total metal content Content 2.33wt%)) at 15 ℃
In 10% concentration hydrochloric acid, washed with stirring for 2 hours, washed thoroughly with water until the aqueous phase becomes neutral, and vacuum dried to give activated carbon C (Si0.46wt%, Al0.1wt%, Fe0.01wt. %, Others 0.001 wt% (total metal content 0.57 wt%).
（２）ホスゲンの製造 スパイラル状にした内径６mm，長さ４ｍのガラス状の反
応管に、上記（１）で得られた活性炭Ｃを３５ｇ充填
し、ガス流入口より一酸化炭素と塩素を等モルの割合
で、かつ両者の混合ガスを１８０g/hr.の流量で導入し
て反応を行った。また、この反応管は、３５０℃に調整
された温度域中に設置した。この際の触媒層の出口温度
は３５２℃であった。(2) Production of phosgene A spiral glass reaction tube having an inner diameter of 6 mm and a length of 4 m is charged with 35 g of the activated carbon C obtained in the above (1), and carbon monoxide and chlorine are supplied from a gas inlet. The reaction was carried out by introducing a mixed gas of both at a molar ratio of 180 g / hr. Moreover, this reaction tube was installed in a temperature range adjusted to 350 ° C. The outlet temperature of the catalyst layer at this time was 352 ° C.
反応後のガスをガスクロマトグラフィーにて分析した結
果、ほぼ１００％の反応率でホスゲンが得られ、またホ
スゲン中の四塩化炭素量は１５０wtppmであった。As a result of analyzing the gas after the reaction by gas chromatography, phosgene was obtained at a reaction rate of almost 100%, and the amount of carbon tetrachloride in phosgene was 150 wtppm.
比較例１ 上記市販の粒状活性炭Ａをそのまま用いたこと以外は、
実施例１（２）と同様の操作を行い、ホスゲンを製造し
た。反応率はほぼ１００％であったが、ホスゲン中の四
塩化炭素量は３８０wtppmと実施例１に比べて２倍以上
に増加していた。Comparative Example 1 Except that the commercially available granular activated carbon A was used as it was,
Phosgene was produced in the same manner as in Example 1 (2). Although the reaction rate was almost 100%, the amount of carbon tetrachloride in phosgene was 380 wtppm, which was more than double that of Example 1.
実施例２ （１）触媒の調製 市販の粒状活性炭Ｂ（直径1.2〜2.4mmに粉砕したヤシ殻
炭；Ｓｉ1.3wt％，Ａｌ1.2wt％，Ｆｅ0.27wt％，その他
0.016wt％（合計金属分含量2.77wt％））を、１５℃で
濃度５％の塩酸に投入し、１時間攪拌洗浄後、水相が中
性になるまで充分に水洗し、真空乾燥して、活性炭Ｄ
（Ｓｉ0.56wt％，Ａｌ0.24wt％，Ｆｅ0.19wt％，その他
0.01wt％（合計金属分含量0.99wt％））を得た。Example 2 (1) Preparation of catalyst Commercially available granular activated carbon B (coconut shell coal crushed to a diameter of 1.2 to 2.4 mm; Si1.3 wt%, Al1.2 wt%, Fe0.27 wt%, others
0.016 wt% (total metal content 2.77 wt%) was added to hydrochloric acid having a concentration of 5% at 15 ° C., washed with stirring for 1 hour, thoroughly washed with water until the aqueous phase became neutral, and vacuum dried. , Activated carbon D
(Si0.56wt%, Al0.24wt%, Fe0.19wt%, others
0.01 wt% (total metal content 0.99 wt%)) was obtained.
（２）ホスゲンの製造 活性炭Ｃの代わりに、上記実施例２（１）で得られた活
性炭Ｄを用いたこと以外は、実施例１（２）と同様の操
作を行い、ホスゲンを製造した。反応率はほぼ１００％
であり、またホスゲン中の四塩化炭素量は２００wtppm
であった。(2) Production of phosgene Phosgene was produced in the same manner as in Example 1 (2) except that the activated carbon D obtained in Example 2 (1) was used instead of the activated carbon C. Reaction rate is almost 100%
And the amount of carbon tetrachloride in phosgene is 200 wtppm
Met.
実施例３ （１）触媒の調製 上記市販の粒状活性炭Ｂを、１５℃で濃度１０％の塩酸
に投入し、１時間攪拌洗浄後、水相が中性になるまで充
分に水洗し、真空乾燥して、活性炭Ｅ（Ｓｉ0.6wt％，
Ａｌ0.07wt％，Ｆｅ0.02wt％，その他0.004wt％（合計
金属分含量0.69wt％））を得た。Example 3 (1) Preparation of catalyst The above-mentioned commercially available granular activated carbon B was placed in hydrochloric acid having a concentration of 10% at 15 ° C., washed with stirring for 1 hour, then sufficiently washed with water until the aqueous phase became neutral, and vacuum dried. And activated carbon E (Si 0.6 wt%,
Al0.07 wt%, Fe0.02 wt% and others 0.004 wt% (total metal content 0.69 wt%) were obtained.
（２）ホスゲンの製造 活性炭Ｃの代わりに、上記実施例３（１）で得られた活
性炭Ｅを用いたこと以外は、実施例１（２）と同様の操
作を行い、ホスゲンを製造した。反応率はほぼ１００％
であり、またホスゲン中の四塩化炭素量は１８０wtppm
であった。(2) Production of phosgene Phosgene was produced in the same manner as in Example 1 (2) except that the activated carbon E obtained in Example 3 (1) was used instead of the activated carbon C. Reaction rate is almost 100%
And the amount of carbon tetrachloride in phosgene is 180 wtppm
Met.
比較例２ 上記市販の粒状活性炭Ｂをそのまま用いたこと以外は、
実施例１（２）と同様の操作を行い、ホスゲンを製造し
た。反応率はほぼ１００％であったが、ホスゲン中の四
塩化炭素量は４００wtppmと実施例２，３に比べて２倍
あるいはそれ以上に増加していた。Comparative Example 2 Except that the above-mentioned commercially available granular activated carbon B was used as it was,
Phosgene was produced in the same manner as in Example 1 (2). Although the reaction rate was almost 100%, the amount of carbon tetrachloride in phosgene was 400 wtppm, which was double or more than that in Examples 2 and 3.
実施例４ 実施例１（２）において、反応管を３５０℃の代わりに
４００℃に調整された温度域中に設置して、触媒層の出
口温度を４０３℃としたこと以外は、実施例１（２）と
同様の操作を行い、ホスゲンを製造した。反応率はほぼ
１００％であり、またホスゲン中の四塩化炭素量は２３
０wtppmであった。Example 4 Example 1 was repeated except that the reaction tube was placed in a temperature range adjusted to 400 ° C. instead of 350 ° C. and the outlet temperature of the catalyst layer was 403 ° C. in Example 1 (2). The same operation as in (2) was performed to produce phosgene. The reaction rate is almost 100%, and the amount of carbon tetrachloride in phosgene is 23%.
It was 0 wtppm.
本発明の方法によれば、特定の金属成分を特定の含量以
下とすることにより四塩化炭素等の副生成物の少ない高
純度のホスゲンを効率よく製造することができる。ま
た、このようにして得られる高純度のホスゲンは、各種
化学品、特にポリカーボネートの製造原料として有効に
利用される。According to the method of the present invention, a high-purity phosgene with a small amount of by-products such as carbon tetrachloride can be efficiently produced by adjusting the content of a specific metal component to a specific content or less. The high-purity phosgene thus obtained is effectively used as a raw material for manufacturing various chemical products, particularly polycarbonate.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特公 昭55−14044（ＪＰ，Ｂ１) 北川外著“活性炭工業”重化学工業通信 社 昭50−６−30． ｐ．51−52 炭素材料科学会編、“活性炭−基礎と応 用”株式会社講談社 1978−９−１ ｐ. 109 ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References Japanese Patent Publication Sho 55-14044 (JP, B1) Kitagawa, et al. “Activated Carbon Industry,” Heavy Chemical Industry News Agency Sho 50-6-30. p. 51-52 Carbon Society of Japan, "Activated Carbon-Basic and Application" Kodansha Co., Ltd. 1978-9-1 p. 109
Claims (1)
反応させてホスゲンを製造する方法において、活性炭を
酸洗浄して得られる、遷移金属、ホウ素、アルミニウム
又は珪素からなる金属成分の合計が1.5重量％以下の活
性炭を使用することを特徴とするホスゲンの製造方法。1. A method for producing phosgene by reacting carbon monoxide with chlorine using activated carbon as a catalyst, the total of metal components comprising transition metal, boron, aluminum or silicon obtained by acid-washing activated carbon. The method for producing phosgene is characterized by using 1.5% by weight or less of activated carbon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63156040A JPH0629129B2 (en) | 1988-06-25 | 1988-06-25 | Method for producing phosgene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63156040A JPH0629129B2 (en) | 1988-06-25 | 1988-06-25 | Method for producing phosgene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH026307A JPH026307A (en) | 1990-01-10 |
| JPH0629129B2 true JPH0629129B2 (en) | 1994-04-20 |
Family
ID=15619004
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63156040A Expired - Lifetime JPH0629129B2 (en) | 1988-06-25 | 1988-06-25 | Method for producing phosgene |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0629129B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996016898A1 (en) * | 1994-12-01 | 1996-06-06 | Idemitsu Petrochemical Co., Ltd. | Process for producing phosgene |
| WO1997030932A1 (en) * | 1996-02-21 | 1997-08-28 | E.I. Du Pont De Nemours And Company | Phosgene manufacturing process |
| WO1998028227A1 (en) * | 1996-12-20 | 1998-07-02 | E.I. Du Pont De Nemours And Company | Phosgene manufacturing process |
| WO2013137297A1 (en) | 2012-03-13 | 2013-09-19 | 出光興産株式会社 | Method for continuous production of polycarbonate |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0912443B1 (en) * | 1996-06-28 | 2001-09-19 | E.I. Du Pont De Nemours And Company | Phosgene manufacturing process |
| US5986037A (en) * | 1996-12-09 | 1999-11-16 | Mitsubishi Chemical Corporation | Polycarbonate resin with a reduced volatile chlorine content and process for producing the same |
| DE19848668A1 (en) * | 1998-10-22 | 2000-04-27 | Bayer Ag | Phosgene with a low tetrachloro-carbon content for production of poly-carbonate or polyester-carbonate, made by ensuring that the gas leaves the phosgene generator at relatively low temperature and pressure |
| US6399823B1 (en) | 2001-04-30 | 2002-06-04 | General Electric Company | Method for producing phosgene |
| JP4704604B2 (en) * | 2001-05-22 | 2011-06-15 | 株式会社ダイヘン | Welding power supply with output control parameter download function |
| JP5319327B2 (en) * | 2009-02-26 | 2013-10-16 | 帝人株式会社 | Method for producing carbonyl chloride |
| CN102060295B (en) * | 2010-11-06 | 2012-08-08 | 青岛科技大学 | Production technology of high purity phosgene with low hydrogen chloride content |
| CN115779882B (en) * | 2022-12-08 | 2024-06-28 | 万华化学集团股份有限公司 | Preparation method and application of activated carbon catalyst for phosgene synthesis |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5514044A (en) * | 1978-07-18 | 1980-01-31 | Tokyo Shibaura Electric Co | Preparation of ultrasoniccwave detecting contacting piece |
-
1988
- 1988-06-25 JP JP63156040A patent/JPH0629129B2/en not_active Expired - Lifetime
Non-Patent Citations (2)
| Title |
|---|
| 北川外著"活性炭工業"重化学工業通信社昭５０−６−３０．ｐ．５１−５２ |
| 炭素材料科学会編、"活性炭−基礎と応用"株式会社講談社１９７８−９−１ｐ．１０９ |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996016898A1 (en) * | 1994-12-01 | 1996-06-06 | Idemitsu Petrochemical Co., Ltd. | Process for producing phosgene |
| WO1997030932A1 (en) * | 1996-02-21 | 1997-08-28 | E.I. Du Pont De Nemours And Company | Phosgene manufacturing process |
| WO1998028227A1 (en) * | 1996-12-20 | 1998-07-02 | E.I. Du Pont De Nemours And Company | Phosgene manufacturing process |
| WO2013137297A1 (en) | 2012-03-13 | 2013-09-19 | 出光興産株式会社 | Method for continuous production of polycarbonate |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH026307A (en) | 1990-01-10 |
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