JPH0149318B2 - - Google Patents
Info
- Publication number
- JPH0149318B2 JPH0149318B2 JP57222146A JP22214682A JPH0149318B2 JP H0149318 B2 JPH0149318 B2 JP H0149318B2 JP 57222146 A JP57222146 A JP 57222146A JP 22214682 A JP22214682 A JP 22214682A JP H0149318 B2 JPH0149318 B2 JP H0149318B2
- Authority
- JP
- Japan
- Prior art keywords
- coal
- catalyst
- liquefaction
- activity
- specific surface
- 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
- 239000003054 catalyst Substances 0.000 claims description 25
- 239000003245 coal Substances 0.000 claims description 21
- 229910001710 laterite Inorganic materials 0.000 claims description 18
- 239000011504 laterite Substances 0.000 claims description 18
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 230000000694 effects Effects 0.000 description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 229910052742 iron Inorganic materials 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 150000003464 sulfur compounds Chemical class 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- WHRZCXAVMTUTDD-UHFFFAOYSA-N 1h-furo[2,3-d]pyrimidin-2-one Chemical compound N1C(=O)N=C2OC=CC2=C1 WHRZCXAVMTUTDD-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 235000006173 Larrea tridentata Nutrition 0.000 description 1
- 244000073231 Larrea tridentata Species 0.000 description 1
- 239000002253 acid 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
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229960002126 creosote Drugs 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical group 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052596 spinel Chemical group 0.000 description 1
- 239000011029 spinel Chemical group 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Landscapes
- Catalysts (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Description
この発明は、触媒として鉄鉱石を使用する石炭
の液化方法に関するものである。
石炭を水素添加の状態下で熱分解することによ
り、液化炭化水素とする石炭の液化方法が知られ
ている。この方法で石炭を液化するには、熱分解
反応を高温高圧下で行なうことと、多量の水素の
添加が必要とされる。
そこで、上記のような反応条件を緩和するため
に、上記熱分解に触媒を使用することが行なわれ
ている。この触媒は、液化活性を有し、安価でか
つ多量に入手し得るものが望まれている。
しかるに、例えばＨ−Coal法で使用されてい
る触媒はCo−Mo系で高価であり、経済的に問題
がある。また、Fe2O3系として鉄鉱石をを触媒と
して使用することも知られているが、鉄鉱石は安
価で多量に供給し得る反面液化活性が低いとされ
ていた。そこで、液化活性を高めるため、補助触
媒として硫黄化合物を添加することが行なわれて
いるが、硫黄化合物を多量に使用すると、その硫
黄分が液化油中に含まれ、液化油の品位を低下さ
せる問題があつた。
そこで、本発明者等は、安価で多量に供給し得
る鉄鉱石中のラテライト鉱につき、石炭液化用触
媒として活性を有するものの条件を調べた。その
結果、ラテライト鉱の含有成分中のAl2O3／SiO2
比と、NiO量、および、ラテライト鉱の比表面積
が、石炭液化用触媒としての活性に大きく影響
し、上記条件を特定範囲のものに選べば、触媒と
して優れた活性をもち、これにより石炭の液化を
効率的に行ない得ることを知見した。
この発明は、上記知見に基いてなされたもので
あつて、石炭に、高温高圧下の状態で水素を添加
し、触媒の存在下でその熱分解を行うことにより
液化する石炭の液化方法において、NiOを0.1〜
3.0重量％含有し、Al2O3／SiO2比が0.5〜3.0であ
つて、50〜100m2／ｇの比表面積を有するラテラ
イト鉱を、前記熱分解の触媒に使用することに特
徴を有するものである。
この発明において、触媒として使用するラテラ
イト鉱の条件を上述のように限定した理由は、次
の通りである。
NiOは、触媒として、芳香族化合物の水素化反
応に活性を示す作用がある。しかし、その含有量
が0.1重量％未満では上述した作用に所望の効果
が得られない。一方、NiOの含有量が3.0重量％
を超えても上述した作用に格別の向上が現われ
ず、逆にニツケル鉱として評価されるためそのコ
ストが高くなる問題が生ずる。従つて、NiOの含
有量は0.1〜3.0重量％の範囲内に限定した。
Al2O3−SiO2は、酸性としての触媒活性を示す
作用がある。しかし、Al2O3／SiO2比が0.5未満で
は上述した作用に所望の効果が得られない。一
方、Al2O3／SiO2比が3.0を超えても上述した作用
に格別の向上が現われず、逆に、アルミナが金属
類とスピネル構造をもつた化合物に変化してその
活性が低下する問題が生ずる。従つて、Al2O3／
SiO2比は、0.5〜3.0の範囲内に限定した。
比表面積は、触媒としてのラテライト鉱の活性
を物理的に高める上において重要な条件であり、
比表面積が50m2／ｇ未満では所望の活性が得られ
ない。一方、比表面積が100m2／ｇを超えると、
試験の結果液化活性が低下することがわかつた。
従つて、比表面積は50〜100m2／ｇの範囲内に限
定した。
次に、この発明を実施例により比較例と共に説
明する。
実施例 １
粒度が60メツシユ以下で、第１表に示す性状の
石炭50ｇを、第２表に示す成分および比表面積の
ラテライト鉱Ａ，Ｂを触媒として使用し、硫黄
0.5ｇの少量クレオソート油100ｇと共によく混合
した上、振盪式オートクレーブに装入した。
This invention relates to a method for liquefying coal using iron ore as a catalyst. A method of liquefying coal into liquefied hydrocarbons by thermally decomposing coal under hydrogenated conditions is known. In order to liquefy coal using this method, it is necessary to carry out the pyrolysis reaction at high temperature and pressure, and to add a large amount of hydrogen. Therefore, in order to ease the reaction conditions as described above, catalysts are used in the thermal decomposition. It is desired that this catalyst has liquefaction activity, is inexpensive, and can be obtained in large quantities. However, the catalyst used in the H-Coal method, for example, is Co-Mo based and expensive, which poses an economical problem. It is also known that iron ore is used as a catalyst in the Fe 2 O 3 system, but iron ore is cheap and can be supplied in large quantities, but on the other hand, it has been thought that the liquefaction activity is low. Therefore, in order to increase the liquefaction activity, sulfur compounds are added as auxiliary catalysts, but if a large amount of sulfur compounds is used, the sulfur content will be included in the liquefied oil, reducing the quality of the liquefied oil. There was a problem. Therefore, the present inventors investigated the conditions for laterite ore in iron ore, which can be supplied in large quantities at low cost, to be active as a catalyst for coal liquefaction. As a result, Al 2 O 3 /SiO 2 in the components of laterite ore
The ratio, the amount of NiO, and the specific surface area of the laterite ore greatly affect the activity as a catalyst for coal liquefaction.If the above conditions are selected within a specific range, the catalyst will have excellent activity, and this will result in a coal liquefaction catalyst. It was discovered that liquefaction can be carried out efficiently. The present invention has been made based on the above findings, and is a coal liquefaction method in which hydrogen is added to coal under high temperature and high pressure, and the coal is liquefied by thermal decomposition in the presence of a catalyst. NiO from 0.1
It is characterized in that laterite ore containing 3.0% by weight, an Al 2 O 3 /SiO 2 ratio of 0.5 to 3.0, and a specific surface area of 50 to 100 m 2 /g is used as the catalyst for the thermal decomposition. It is something. In this invention, the reason why the conditions for the laterite ore used as a catalyst are limited as described above is as follows. NiO acts as a catalyst, showing activity in the hydrogenation reaction of aromatic compounds. However, if the content is less than 0.1% by weight, the desired effects described above cannot be obtained. Meanwhile, the content of NiO is 3.0% by weight
Even if it exceeds 100%, the above-mentioned effect will not be significantly improved, and on the contrary, it will be evaluated as nickelite, resulting in the problem of increased cost. Therefore, the content of NiO was limited within the range of 0.1 to 3.0% by weight. Al 2 O 3 -SiO 2 has the effect of exhibiting catalytic activity as an acid. However, if the Al 2 O 3 /SiO 2 ratio is less than 0.5, the desired effect described above cannot be obtained. On the other hand, even if the Al 2 O 3 /SiO 2 ratio exceeds 3.0, no particular improvement in the above-mentioned effects appears; on the contrary, alumina changes into a compound with metals and a spinel structure, and its activity decreases. A problem arises. Therefore, Al 2 O 3 /
The SiO2 ratio was limited to a range of 0.5 to 3.0. The specific surface area is an important condition for physically increasing the activity of laterite ore as a catalyst.
If the specific surface area is less than 50 m 2 /g, the desired activity cannot be obtained. On the other hand, when the specific surface area exceeds 100m 2 /g,
As a result of the test, it was found that the liquefaction activity decreased.
Therefore, the specific surface area was limited to a range of 50 to 100 m 2 /g. Next, the present invention will be explained based on examples and comparative examples. Example 1 50 g of coal with a particle size of 60 mesh or less and properties shown in Table 1 was converted into sulfur using laterite ores A and B having the components and specific surface areas shown in Table 2 as catalysts.
A small amount of 0.5 g was mixed well with 100 g of creosote oil, and the mixture was charged into a shaking autoclave.
【表】【table】
【表】
次いで、水素初圧80Kg／cm2、温度400℃、反応
時間60分の条件で水素添加後、内容物の抽出試験
およびガス分析を行なつた。第３表はその結果で
テトラヒドロフラン（THF）抽出後の液化率は、
触媒としてラテライト鉱Ａを使用した場合は95.4
％、ラテライト鉱Ｂを使用した場合は93.4％であ
り、油中のヘキサン可溶分は、ラテライト鉱Ａを
使用した場合は39.0％、ラテライト鉱Ｃを使用し
た場合は32.4％であつて極めて高い値を示した。
なお、ここで液化率とは、石炭中の揮発分と固定
炭素とに含有されている炭素を100としたときの
液体炭化水素の回収率である。[Table] Next, after hydrogenation was performed under the conditions of an initial hydrogen pressure of 80 Kg/cm 2 , a temperature of 400° C., and a reaction time of 60 minutes, an extraction test and gas analysis of the contents were performed. Table 3 shows the results, and the liquefaction rate after extraction with tetrahydrofuran (THF) is
95.4 when laterite ore A is used as a catalyst
%, when laterite ore B is used, it is 93.4%, and the hexane soluble content in the oil is 39.0% when laterite ore A is used, and 32.4% when laterite ore C is used, which is extremely high. The value was shown.
Note that the liquefaction rate here refers to the recovery rate of liquid hydrocarbons when the carbon contained in the volatile matter and fixed carbon in the coal is taken as 100.
【表】
実施例 ２
実施例１と同一の石炭に対し、同じく実施例１
と同一のラテライト鉱を触媒として使用し、硫黄
の添加は行なわずに、他は実施例１と同一の条件
で液化処理を行なつた。第４表にそのときの結果
を示す。[Table] Example 2 For the same coal as in Example 1,
The liquefaction treatment was carried out under the same conditions as in Example 1, using the same laterite ore as the catalyst and without adding sulfur. Table 4 shows the results.
【表】
比較例
実施例１と同一の石炭に対し、第５表に示す成
分および比表面積のラテライト鉱Ｃ，Ｄを使用
し、他は実施例１と同一の条件で液化処理を行な
つた。第６表にそのときの結果を示す。[Table] Comparative example The same coal as in Example 1 was subjected to liquefaction treatment using laterite ores C and D having the components and specific surface areas shown in Table 5, and under the same conditions as in Example 1. . Table 6 shows the results.
【表】【table】
【表】
上記第３表および第６表から明らかなように、
NiO含有量、Al2O3／SiO2比および比表面積が本
発明範囲内のラテライト鉱Ａ，Ｂを触媒として使
用した場合は、上記条件が本発明範囲外のラテラ
イト鉱Ｃ，Ｄと比較して、優れた液化率およびヘ
キサン可溶分を示した。
この発明において触媒として使用される鉄鉱石
のラテライト鉱は、塩基性火成岩が風化分解して
２次的に生成したもので、Fe：40〜50wt％、
Al2O3：５〜15％のほか、Cr，Ni，Mo等を不純
物としてそれぞれ１％前後含有する成分組成を有
する多孔質または土状の褐鉄鉱であり、熱帯地方
に広く分布し、その埋蔵量は約200憶屯と云われ
る莫大な量であるから、安価にかつ多量に入手す
ることができる。
以上述べたように、この発明によれば、触媒と
して安価でかつ多量に入手でき、しかも活性に優
れているラテライト鉱の如き低品位鉄鉱石を使用
することにより、硫黄化合物の如き補助触媒を要
せずまたは少量の使用で、高い効率で石炭の液化
を行なうことができる工業上優れた効果がもたれ
される。[Table] As is clear from Tables 3 and 6 above,
When laterite ores A and B whose NiO content, Al 2 O 3 /SiO 2 ratio and specific surface area are within the range of the present invention are used as catalysts, compared with laterite ores C and D where the above conditions are outside the range of the present invention. It showed excellent liquefaction rate and hexane soluble content. The laterite ore of iron ore used as a catalyst in this invention is a secondary product produced by weathering and decomposition of basic igneous rock, Fe: 40 to 50 wt%,
Al 2 O 3 : Porous or earthy limonite with a component composition containing 5 to 15% and impurities such as Cr, Ni, and Mo at around 1% each. It is widely distributed in tropical regions, and has large reserves. The amount is said to be about 200 million tons, so it can be obtained at low cost and in large quantities. As described above, according to the present invention, by using low-grade iron ore such as laterite ore, which is inexpensive and available in large quantities and has excellent activity, as a catalyst, an auxiliary catalyst such as a sulfur compound is not required. It is possible to liquefy coal with high efficiency without using it or with a small amount, and it has an excellent industrial effect.
Claims (1)
触媒の存在下でその熱分解を行なうことによりこ
れを液化する石炭の液化方法において、 NiOを0.1〜3.0重量％含有し、Al2O3／SiO2比
が0.5〜3.0であつて、50〜100m2／ｇの比表面積
を有するラテライト鉱を、前記熱分解の触媒に使
用することを特徴とする石炭の液化方法。[Claims] 1. Hydrogen is added to coal under high temperature and high pressure,
In a method for liquefying coal by thermally decomposing it in the presence of a catalyst, the coal contains 0.1 to 3.0% by weight of NiO, the Al 2 O 3 /SiO 2 ratio is 0.5 to 3.0, and the coal is liquefied by thermal decomposition in the presence of a catalyst. A method for liquefying coal, characterized in that laterite ore having a specific surface area of 100 m 2 /g is used as a catalyst for the thermal decomposition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22214682A JPS59113090A (en) | 1982-12-20 | 1982-12-20 | Liquefaction of coal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22214682A JPS59113090A (en) | 1982-12-20 | 1982-12-20 | Liquefaction of coal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59113090A JPS59113090A (en) | 1984-06-29 |
| JPH0149318B2 true JPH0149318B2 (en) | 1989-10-24 |
Family
ID=16777895
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP22214682A Granted JPS59113090A (en) | 1982-12-20 | 1982-12-20 | Liquefaction of coal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59113090A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH073821U (en) * | 1993-06-21 | 1995-01-20 | 株式会社東洋工機 | Press brake |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6183284A (en) * | 1984-09-29 | 1986-04-26 | Nippon Kokan Kk <Nkk> | Liquefaction of coal |
| JPS6183287A (en) * | 1984-09-29 | 1986-04-26 | Nippon Kokan Kk <Nkk> | Liquefaction of coal |
| JPS6183285A (en) * | 1984-09-29 | 1986-04-26 | Nippon Kokan Kk <Nkk> | Liquefaction of coal |
| JPS6183286A (en) * | 1984-09-29 | 1986-04-26 | Nippon Kokan Kk <Nkk> | Liquefaction of coal |
| JPS6183288A (en) * | 1984-09-29 | 1986-04-26 | Nippon Kokan Kk <Nkk> | Liquefaction of coal |
| JP5102934B2 (en) * | 2004-05-19 | 2012-12-19 | 株式会社ロッテ | New liquor |
| CN104607192A (en) * | 2015-01-23 | 2015-05-13 | 上海大学 | Coal electrolysis hydro-liquefaction catalyst and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55116793A (en) * | 1979-03-02 | 1980-09-08 | Mitsubishi Chem Ind Ltd | Method of coal liquefaction |
| JPS55123682A (en) * | 1979-03-16 | 1980-09-24 | Mitsubishi Chem Ind Ltd | Liquefaction of coal |
-
1982
- 1982-12-20 JP JP22214682A patent/JPS59113090A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55116793A (en) * | 1979-03-02 | 1980-09-08 | Mitsubishi Chem Ind Ltd | Method of coal liquefaction |
| JPS55123682A (en) * | 1979-03-16 | 1980-09-24 | Mitsubishi Chem Ind Ltd | Liquefaction of coal |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH073821U (en) * | 1993-06-21 | 1995-01-20 | 株式会社東洋工機 | Press brake |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS59113090A (en) | 1984-06-29 |
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