JPH0450957B2 - - Google Patents
Info
- Publication number
- JPH0450957B2 JPH0450957B2 JP25892684A JP25892684A JPH0450957B2 JP H0450957 B2 JPH0450957 B2 JP H0450957B2 JP 25892684 A JP25892684 A JP 25892684A JP 25892684 A JP25892684 A JP 25892684A JP H0450957 B2 JPH0450957 B2 JP H0450957B2
- Authority
- JP
- Japan
- Prior art keywords
- crude phenol
- water
- crude
- phenol
- mirabilite
- 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
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 43
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 34
- 239000010446 mirabilite Substances 0.000 claims description 31
- 239000011289 tar acid Substances 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 16
- 238000000354 decomposition reaction Methods 0.000 claims description 15
- 238000011084 recovery Methods 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 10
- RSIJVJUOQBWMIM-UHFFFAOYSA-L sodium sulfate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]S([O-])(=O)=O RSIJVJUOQBWMIM-UHFFFAOYSA-L 0.000 claims description 10
- 239000011280 coal tar Substances 0.000 claims description 8
- 230000018044 dehydration Effects 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- ISWSIDIOOBJBQZ-UHFFFAOYSA-M phenolate Chemical compound [O-]C1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-M 0.000 claims description 8
- 229940031826 phenolate Drugs 0.000 claims description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 21
- 238000000034 method Methods 0.000 description 14
- 238000011282 treatment Methods 0.000 description 6
- 238000007796 conventional method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005185 salting out Methods 0.000 description 3
- 239000010802 sludge Substances 0.000 description 3
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Landscapes
- Working-Up Tar And Pitch (AREA)
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、コールタールからのタール酸の製造
方法に関し、更に詳しくは、タール酸の回収率を
向上させるための方法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method for producing tar acid from coal tar, and more particularly to a method for improving the recovery rate of tar acid.
従来の技術及びその問題点
従来、コールタールからのタール酸の製造方法
としては、第１図のフローチヤートに示すような
方法が知られている。第１図に示す方法では、ま
ず、コールタールを蒸留して得られるカルボン油
及びナフタリン油に苛性ソーダを添加して脱酸す
ることにより、粗フエノレートを得る。次いで、
この粗フエノレートにスチームによるダンピング
処理を行なうことにより、中性分、塩基分などの
不純物を除去した後、硫酸分解して粗フエノール
とする。次いで、水洗、脱水処理後粗フエノール
を蒸留することによりタール酸製品を得ることが
できる。BACKGROUND ART AND PROBLEMS Conventionally, as a method for producing tar acid from coal tar, a method as shown in the flowchart of FIG. 1 is known. In the method shown in FIG. 1, first, crude phenolate is obtained by adding caustic soda to carbon oil and naphthalene oil obtained by distilling coal tar to deoxidize them. Then,
This crude phenolate is subjected to a damping treatment with steam to remove impurities such as neutral components and base components, and then decomposed with sulfuric acid to obtain crude phenol. Next, a tar acid product can be obtained by distilling the crude phenol after washing with water and dehydration.
しかしながら、このタール酸の製造方法では以
下に示す問題点により、タール酸の回収率が満足
いくものではない。 However, in this method for producing tar acid, the recovery rate of tar acid is not satisfactory due to the following problems.
イ硫酸分解後に、粗フエノールと芒硝とを比重差
により分離する過程において、芒硝側に粗フエ
ノールが同伴する。After the decomposition of isulfuric acid, in the process of separating crude phenol and mirabilite based on the difference in specific gravity, crude phenol is entrained on the mirabilite side.
ロ 粗フエノールの水洗後、比重差により、粗フ
エノールと水とを分離する過程において、水側
に多くの粗フエノールが含まれる。(b) After washing the crude phenol with water, in the process of separating the crude phenol from water due to the difference in specific gravity, a large amount of crude phenol is contained on the water side.
ハ 水洗後の蒸発脱水工程で水に多くのフエノー
ルが同伴する。C. A large amount of phenol is entrained in water during the evaporation and dehydration process after washing with water.
また、このように上記イ）〜ハ）により得られ
る芒硝及び水が粗フエノールを多く含むものであ
ることから、従来はこの芒硝及び水は、芒硝を回
収した後、又は回収することなく活性汚泥法によ
り廃水処理を施されているが、この処理量が多
く、かつ処理負荷が高いという問題もある。 In addition, since the mirabilite and water obtained in steps a) to c) above contain a large amount of crude phenol, conventionally, the mirabilite and water were processed by the activated sludge method after or without recovering the mirabilite. Although wastewater treatment is being carried out, there are also problems in that the amount of wastewater to be treated is large and the processing load is high.
問題点を解決するための方法
本発明者は、コールタールからタール酸の製造
する方法において、タール酸の回収率を向上させ
るための方法を見出すべく鋭意研究を重ねた結
果、硫酸分解後に粗フエノールから分離された芒
硝、粗フエノールの水洗水、及び粗フエノールの
脱水により得られる水を回収し、混合して静置す
ることにより、塩析効果により粗フエノールと芒
硝水との分離が良好となり、効率的な粗フエノー
ルの回収がはかれることを見出した。本発明は、
この知見に基づくものである。Method for Solving the Problems As a result of intensive research to find a method for improving the recovery rate of tar acid in a method for producing tar acid from coal tar, the present inventor found that crude phenol was recovered after decomposition with sulfuric acid. By collecting the water obtained by dehydrating the crude phenol, the water obtained by washing the mirabilite separated from the mirabilite, and the water obtained by dehydrating the crude phenol, the crude phenol and the mirabilite water can be separated well due to the salting out effect. It has been found that crude phenol can be efficiently recovered. The present invention
It is based on this knowledge.
即ち、本発明は、コールタール由来の粗フエノ
レートからタール酸を製造するに際し、
硫酸分解後に得られる芒硝、
硫酸分解後の粗フエノールの水洗水、及び
粗フエノールの蒸発脱水により得られる水
を回収セパレーター中で混合し、静置して、分離
した粗フエノールを回収し、硫酸分解後の粗フエ
ノールとともに水洗工程を供することを特徴とす
るタール酸の製造法に係る。 That is, the present invention, when producing tar acid from crude phenolate derived from coal tar, uses a separator to collect the mirabilite obtained after decomposition with sulfuric acid, the washing water of the crude phenol after decomposition with sulfuric acid, and the water obtained by evaporative dehydration of the crude phenol. This relates to a method for producing tar acid, which is characterized in that the crude phenol is mixed in a container, allowed to stand, and separated crude phenol is recovered, and subjected to a water washing step together with the crude phenol after decomposition with sulfuric acid.
本発明によるタール酸の製造方法のフローチヤ
ートを第２図に示す。 A flowchart of the method for producing tar acid according to the present invention is shown in FIG.
本発明方法では、まずコールタールに、従来法
と同様に、蒸留、脱酸、ダンピング。硫酸分解の
各処理を行なうことにより、粗フエノールを得
る。硫酸分解までの処理条件は、従来方法と同様
でよく、特殊な条件は必要とされない。 In the method of the present invention, coal tar is first subjected to distillation, deoxidation, and dumping in the same manner as in the conventional method. Crude phenol is obtained by performing each treatment of sulfuric acid decomposition. The processing conditions up to sulfuric acid decomposition may be the same as those of conventional methods, and no special conditions are required.
硫酸分解後は、粗フエノールと芒硝とを比重差
により分離させる。得られる芒硝は、0.6〜１％
程度の粗フエノールを同伴するものであり、回収
セパレーターに送られる。 After decomposition with sulfuric acid, crude phenol and Glauber's salt are separated based on the difference in specific gravity. The obtained mirabilite is 0.6-1%
It is accompanied by some crude phenol and is sent to the recovery separator.
硫酸分解後の粗フエノールは、芒硝を少量含む
ため、水洗により芒硝の除去を行なう。水洗水
は、比重差により粗フエノールから分離される
が、水側には、３〜５％程度の粗フエノールが含
まれるので水洗水は回収セパレーターに送られ
る。 Since the crude phenol after decomposition with sulfuric acid contains a small amount of Glauber's salt, the Glauber's salt is removed by washing with water. The washing water is separated from the crude phenol due to the difference in specific gravity, but since the water side contains about 3 to 5% crude phenol, the washing water is sent to the recovery separator.
水洗後の粗フエノールは、蒸発脱水による水分
を除去される。蒸発脱水により得られる水には、
３〜６％程度の粗フエノールが含まれるので、こ
の水も回収セパレーターに送られる。 The water content of the crude phenol after washing with water is removed by evaporation and dehydration. Water obtained by evaporative dehydration includes
Since it contains approximately 3-6% crude phenol, this water is also sent to the recovery separator.
次いで蒸発脱水した粗フエノールを常法に従つ
て蒸留することによりタール酸製品が得られる。 The evaporated and dehydrated crude phenol is then distilled in a conventional manner to obtain a tar acid product.
回収セパレーターでは、硫酸分解後に粗フエノ
ールから分離された芒硝、粗フエノールの水洗
水、及び粗フエノールの蒸発脱水により得られる
水を混合し、静置する。この回収した混合物中に
は、芒硝が多量に含まれるため塩析効果により、
粗フエノールが容易に芒硝水から分離する。回収
セパレーターでは芒硝濃度や、粗フエノール濃度
等により条件は異なるが、通常は温度40〜80℃程
度で0.5〜1.0時間程度静置すればよい。 In the recovery separator, the mirabilite separated from the crude phenol after decomposition with sulfuric acid, the washing water of the crude phenol, and the water obtained by evaporative dehydration of the crude phenol are mixed and allowed to stand. This recovered mixture contains a large amount of Glauber's salt, so due to the salting out effect,
Crude phenol is easily separated from the mirabilite solution. Conditions for the recovery separator vary depending on the concentration of Glauber's salt, the concentration of crude phenol, etc., but usually it is sufficient to leave it standing at a temperature of about 40 to 80°C for about 0.5 to 1.0 hours.
回収した粗フエノールは、硫酸分解処理後に得
られる粗フエノールとともに水洗工程に送られ、
タール酸の製造に利用される。 The recovered crude phenol is sent to a water washing process together with the crude phenol obtained after sulfuric acid decomposition treatment.
Used in the production of tar acid.
粗フエノールと芒硝水とに分離前の回収混合物
中には0.8〜1.5％程度の粗フエノールが含まれる
が、塩析効果を利用して粗フエノールを分離した
後の芒硝水は0.6％程度の粗フエノールを含むの
みである。従つて粗フエノールの回収率が向上す
るとともに、芒硝水から芒硝を回収した後、また
は芒硝を回収することなく活性汚泥処理を行なう
場合に、処理負荷を低減できるという利点もあ
る。 The recovered mixture before separation into crude phenol and Glauber's salt water contains approximately 0.8 to 1.5% crude phenol, but after separating the crude phenol using the salting out effect, the Glauber's salt water contains approximately 0.6% crude phenol. Contains only phenol. Therefore, the recovery rate of crude phenol is improved, and there is also the advantage that the processing load can be reduced when activated sludge treatment is performed after recovering mirabilite from mirabilite water or without recovering mirabilite.
発明の効果
本発明方法によれば、粗フエノールの回収率を
向上させることができることにより、タール酸製
品の収率が向上する。また、廃水中に含まれる粗
フエノールが減少することにより、活性汚泥処理
負荷の低減がはかれる。Effects of the Invention According to the method of the present invention, the recovery rate of crude phenol can be improved, thereby improving the yield of tar acid products. Furthermore, by reducing the amount of crude phenol contained in wastewater, the load on activated sludge treatment can be reduced.
実施例
以下に実施例を示して本発明を詳細に説明す
る。EXAMPLES The present invention will be described in detail with reference to Examples below.
実施例 １
常法に従つてコールタールに蒸留、脱酸、ダン
ピングの各処理を行なつて酸性分を20％含む粗フ
エノレートを得た。Example 1 Coal tar was subjected to distillation, deacidification, and dumping treatments according to conventional methods to obtain crude phenolate containing 20% acidic content.
この粗フエノレートを原料として第３図に示す
フローチヤートに従つて、以下に示す方法で粗フ
エノレートの処理量50t／日として、粗フエノー
ルの製造及び回収を行なつた。まず粗フエノレー
ト50t／日に66％硫酸7.1t／日を加えて、硫酸分
解し、芒硝と粗フエノールとに分離させた。この
芒硝には、粗フエノールが0.4t／日同伴され、粗
フエノールは芒硝を含む水1.8t／日を同伴してい
た。次いで粗フエノールを水5.7t／日で水洗し
て、水1.8t／日を含む粗フエノール9.4t／日と粗
フエノール0.2t／日を含む水洗水5.7t／日（粗フ
エノール分3.4％）とを得た。次いでこの水を含
む粗フエノールを蒸発脱水して、水0.2t／日を含
む粗フエノール9.8t／日と粗フエノール0.1t／日
を含む水1.6t／日（粗フエノール分5.8％）とに分
離させた。 Using this crude phenolate as a raw material, crude phenol was produced and recovered in accordance with the flowchart shown in FIG. 3 in the following manner at a throughput of 50 tons/day. First, 7.1 t/day of 66% sulfuric acid was added to 50 t/day of crude phenolate to decompose it with sulfuric acid and separate it into Glauber's salt and crude phenol. This mirabilite was accompanied by 0.4 t/day of crude phenol, and the crude phenol was accompanied by 1.8 t/day of water containing mirabilite. Next, the crude phenol was washed with 5.7 t/day of water to obtain 9.4 t/day of crude phenol containing 1.8 t/day of water and 5.7 t/day of washing water containing 0.2 t/day of crude phenol (crude phenol content: 3.4%). I got it. The crude phenol containing water is then evaporated and dehydrated to separate it into 9.8 t/day of crude phenol containing 0.2 t/day of water and 1.6 t/day of water (crude phenol content 5.8%) containing 0.1 t/day of crude phenol. I let it happen.
硫酸分解により得た粗フエノールを含む芒硝、
及び水洗、脱水工程で得た粗フエノールを含む水
を回収セパレーターに集めて混合し、静置させ
た。静置により粗フエノールと芒硝水とに分離
し、0.4t／日の粗フエノールを回収することがで
きた。 Glauber's salt containing crude phenol obtained by sulfuric acid decomposition;
The water containing crude phenol obtained in the water washing and dehydration steps was collected in a recovery separator, mixed, and allowed to stand still. By allowing the mixture to stand still, it was separated into crude phenol and mirabilite water, and 0.4 t/day of crude phenol could be recovered.
また芒硝水には、0.3t／日の粗フエノールが含
まれるだけであり、芒硝水中の粗フエノール分
は、0.6％と低減した。 In addition, the mirabilite solution contained only 0.3 t/day of crude phenol, and the crude phenol content in the mirabilite solution was reduced to 0.6%.
以上の結果から明らかなごとく、本発明方法で
は、従来法と比較して粗フエノールの回収量が
0.4t／日増加し、芒硝水中の粗フエノール分は、
粗フエノール回収前は、1.3％であつたものが、
粗フエノール回収後は、0.6％に低減した。 As is clear from the above results, the amount of crude phenol recovered in the method of the present invention is lower than that in the conventional method.
The crude phenol content in mirabilite water increased by 0.4t/day.
Before crude phenol recovery, it was 1.3%;
After recovering crude phenol, it was reduced to 0.6%.
第１図は、従来法によるタール酸製造プロセス
のフローチヤート、第２図は、本発明方法による
タール酸製造プロセスのフローチヤートである。
第３図は、実施例１の粗フエノレートから粗フエ
ノールを製造する工程のフローチヤートである。
FIG. 1 is a flowchart of a tar acid production process according to a conventional method, and FIG. 2 is a flowchart of a tar acid production process according to a method of the present invention.
FIG. 3 is a flowchart of the process of producing crude phenol from the crude phenolate of Example 1.
Claims (1)
ル酸を製造するに際し、 硫酸分解後に得られる芒硝、 硫酸分解後の粗フエノールの水洗水、及び 粗フエノールの蒸発脱水により得られる水、 を回収セパレーター中で混合し、静置して、分離
した粗フエノールを回収し、硫酸分解後の粗フエ
ノールとともに水洗工程に供することを特徴とす
るタール酸の製造法。[Scope of Claims] 1. In producing tar acid from crude phenolate derived from coal tar, the following are prepared: Glauber's salt obtained after decomposition with sulfuric acid, water for washing the crude phenol after decomposition with sulfuric acid, and water obtained by evaporative dehydration of the crude phenol. A method for producing tar acid, which comprises mixing in a recovery separator, allowing it to stand, and recovering the separated crude phenol, which is then subjected to a water washing process together with the crude phenol after decomposition with sulfuric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25892684A JPS61136589A (en) | 1984-12-06 | 1984-12-06 | Preparation of tar acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25892684A JPS61136589A (en) | 1984-12-06 | 1984-12-06 | Preparation of tar acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61136589A JPS61136589A (en) | 1986-06-24 |
| JPH0450957B2 true JPH0450957B2 (en) | 1992-08-17 |
Family
ID=17326955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25892684A Granted JPS61136589A (en) | 1984-12-06 | 1984-12-06 | Preparation of tar acid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61136589A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018198428A1 (en) * | 2017-04-26 | 2018-11-01 | Ｊｆｅケミカル株式会社 | Method for recovering tar acid salt and method for producing tar acid |
| CN109604307A (en) * | 2018-12-07 | 2019-04-12 | 山西焦化股份有限公司 | A kind of equipment that two recovery systems crude benzol regeneration slag recycles |
-
1984
- 1984-12-06 JP JP25892684A patent/JPS61136589A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61136589A (en) | 1986-06-24 |
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