WO1984000558A1 - Process for removing quinoline insolubles from topped tar - Google Patents

Abstract

Quinoline insolubles (QI) are removed by centrifuging topped tar or a mixture of topped tar with coal tar gas oil or middle oil at high temperatures.

Description

 Akira

 Quinoline insolubles from tar when

 How to remove

 The present invention provides a method for removing quinoline-insoluble matter from extracted tar (hereinafter simply referred to as “quinoline

 §8 to remove QI).

 In the specification and the scope of the present application, the term “out-of-head tar” refers to a component which is obtained by distilling a coal tar and having a point lower than the degree of action at the time of arrest and separation. What did you do?

 When high-quality carbon materials such as needle coke and carbon fiber are produced using coal tar as a starting material, QI, which is a consumable in the coal tar, can be produced. Only need to be removed. The QI component is a carbonaceous particle having a diameter of 0.3 ia or less, and when contained in a large amount in the coal tar, the mesophase (sphere) is formed in the mature process of the coal tar. It is believed that it adheres to the surface of S) to prevent coalescence of the spheres S and impairs the smooth growth of spherulites.

 For this reason, the necessity of removing the QI component in the coal tar has been conventionally recognized. For example, the following method has been implemented. That is, an oil having poor mutual solubility with the coal tar, for example, a petroleum light oil is added to the coal tar.

After coagulating and sedimenting the QI component to increase the particle size of the QI component,

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, WIPO There is a method for sedimentation of the QI component that is large in IE (Japanese Patent Publication No. 52-28501). In this method, it is necessary to obtain the useful components such as tar and Z or pitch and to recover the S-added oil by steaming the clarified liquid after the QI separation. This not only requires a large amount of ripening energy, but also decreases the yield of useful components.β Furthermore, the oil recovered by steaming g It is a mixture with stone-based oil derived from it, and its utility is low until then. On the other hand, the sedimentation phase separated by the silence contains a large amount of petroleum-based oil, and if no recovery treatment is carried out, the recovery rate of the added oil will be low, and the recovery rate will be lower. For such treatment, equipment such as a steam bud tower and tanks will be required. In addition, large tanks for preserving petroleum-based light and medium oils to be added, and other auxiliary facilities are required, and a vast installation area is also required.

 Restatement of invention

 The inventor of the present invention has conducted various studies to solve or eliminate the above-mentioned problems of the conventional method, and as a result, has found that a call-tar-based light can be added to the extracted tar or the ring-extracted tar. It was found that the QI component was easily and efficiently separated by subjecting the s-compound to which the medium oil was added to sa centrifugation. Around this time, it was completed based on these findings.

 According to the method of the present invention, it is not always necessary to use a solvent.

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, Small V / ΙΡϋ ^ Also, when used, the solvent is made of coal tar, so the oil recovered by centrifugal sea bass steaming consists only of the coal tar and can be used effectively. It is. Furthermore, it is not necessary to conceal the sedimentation phase g and does not need a large amount of ripening energy for the steam S. In addition, a remarkable effect is obtained in that the yield of tar and pho or pit is remarkably high.

 In the method of the present invention, the exfoliated tar obtained by steam SB of the coal tar is subjected to centrifugal sea bass under the conditions of 100 to 400. When the temperature is lower than 100, it is difficult to sufficiently remove QI, and when the temperature is higher than 400, gas generation and tar alteration due to thermal decomposition of tar occur. « The S degree at the time of centrifugation is more preferably 200 to 350. As the centrifuge, various types of concealment that can be operated within the above-mentioned a degree range can be used. The centrifugal force is usually

It is about 500-3500G, and more preferably about 2000-3500G. The removal rate of QI may be appropriately determined according to the properties of the tar when the raw material is removed, the type of the final product, and the like. For example, in order to obtain a raw coke raw material from a head with a QI content of 3.596, the QI content removal rate is preferably 90% or more, and a carbon fiber raw material is obtained. For this purpose, it is preferable that the QI component removal rate be 9 596 or more. If necessary, the clarified liquid after the stern is steamed according to a conventional method, and then further processed to obtain a final product. In the method of the present invention, it is possible to add a coal-tar light-medium oil to the tar at the time of removal. Thus, since the viscosity of 9ι tar drops, not only can the operation severity be reduced to 80 to 300, but also the QI removal effect by centrifugation is improved. It will be possible to do so. Examples of the coal-tar light-medium oil to be used include creator oil, naphthalene oil, and anthracene oil having a boiling point of about 80 to 350. It is preferable to use about 20 to 200 parts by weight of the coal tar-based light / medium oil per 100 parts by weight of the extracted tar. More preferably, it is about 50 parts by weight. By distilling the clarified liquid from which a predetermined amount of QI has been removed by 18 centrifuges, the desired raw material for carbon material can be obtained in S yield, and the coal tar oil is recovered. . The recovered oil can be used again as an added oil to the exfoliation tar. In addition, when adding a coal tar light medium oil to the extraction tar, it is more preferable to set the operating temperature during centrifugation to 100 to 250.

 According to the method of the present invention, the following effects are obtained.

 (a) The QI component in the excavated tar is easily and efficiently removed, and a useful component (tall or pitch) with a low QI content can be obtained at an S ぃ yield.

 () It is not always necessary to use a solvent.

(c) When a solvent is used, it is light and medium Three

 Since oil is used, the oil collected by the centrifugal shunter steam S consists solely of a coal tar system, and is effectively used as it is.

 (d) Ripe energy consumption is low.

 (e) There is no need for crabs for sedimentation phase distillation or large tanks for storing oils obtained from sedimentation phase steam S.

 Examples will be shown below to clarify the features of the present invention.

Real example 1

 Extracted tar obtained by steaming the coal tar with 250)

 (QI content 2.48 weight 6) was centrifuged at S degrees shown in Table 1 below to obtain the QI removal results shown in the table.

 Centrifugal separator capacity is 1 2, rotation speed 4 60.0 rpsi, centrifugal force

 2 500 G, 10 minutes of processing time.

 Table 1

実旌傍 2

Jeongjeungbye 2

 Extracted tar obtained by distilling the coal tar at 250

_ OMPI ¾ ^ s

 (QI content: 2.48 weight: 96) was centrifuged at the concentration shown in Table 2 below to obtain Q 〖removal results shown in the table.

 The centrifugal separator used was a multifilament centrifugal extractor equipped with four 500 W capacity containers, with a rotation speed of 3000 mm fiber, a centrifugal force of 1300 G, and a processing time of 10 min. .

Real example 3

 Extracted tar obtained by distilling the coal tar at 150

 (QI content: 2.0 weight 6> 100 weight; SB) Add naphtholine oil '50 weight »with boiling point of 190-320» to SB and centrifuge under the same conditions The results are as shown in Table 2.

 Table 2

実施例 4

Example 4

Extraction tar similar to that of the side 1 100 A predetermined amount of creosole oil with a boiling point of 190 to 320 was added to Fiber S 100, and centrifuged. The results are as shown in Table 3.

 The centrifugal separation machine used the multi-spin centrifugal stern used in ¾3. The operating conditions were as follows: rotation speed: 3 000 rp, centrifugal force: 1300 G »80 degrees, processing time: ¾1 It was 0 minutes.

 Table 3

実旃钾 5

Real shawl 钾 5

 Excellent tar obtained by distilling the call tar at 200

 <QI content 2.1 weight 96> was centrifuged at the humidity shown in Table 4 below to obtain the results shown in the following table.

As the eccentric centrifugal separator, a horizontal centrifugal centrifugal separator with a holding volume of 40 e was used, the rotation speed was 300,000 rpa, and the centrifugal force was 2,280 G. The throughput was 1 ton / hr. a

 Table 4

第 4 表に示す桔果から 、 本発明方法に よれば、 抜頭タ ー ルに対する Q Ϊ 分除去後の有用成分の収率が極めて高いこ とが明 らかである。

From the results shown in Table 4, it is clear that according to the method of the present invention, the yield of the useful component after removing the Q component from the exfoliated tar is extremely high.

Claims

The scope of the claims  (1) A method for removing quinoline-insoluble components from an exfoliated tar, which is characterized in that the sterilized tar is centrifuged at 100-400. ② The centrifugation is performed at 150-300 ° C.  ③ Perform centrifugation with a quick-force of 500 to 3 ^ 00 G.  加 え Add quintalin-based light-and-medium oil to the exfoliated tar and subject it to quinoline-insoluble matter from the exfoliated tar, which is characterized in that it is subjected to rapid centrifugal separation at 80-300. How to remove.  行 な う The method described in Paragraph 4 of the scope of the lecture, in which the centrifugal separation is performed at 100 to 250.  行 な う The centrifugation is performed with a centrifugal force of 500 to 300 G.  方法 The method according to claim 4, wherein the boiling point of the coal tar light-medium oil is 80 to 350.  ⑧ ¾ ¾ 重量 100 重量 Weight »タ タ 軽 軽 中 中 中 中 軽  The method according to item 4 to the scope of the course of adding 20 to 200 weight 2%.  ⑨ Extraction tar 100% by weight of coal tar light medium oil  The method according to claim 8, wherein the amount of 50 to 150 is added.