GB1598376A - Process for the liquefaction of coal - Google Patents
Process for the liquefaction of coal Download PDFInfo
- Publication number
- GB1598376A GB1598376A GB8579/78A GB857978A GB1598376A GB 1598376 A GB1598376 A GB 1598376A GB 8579/78 A GB8579/78 A GB 8579/78A GB 857978 A GB857978 A GB 857978A GB 1598376 A GB1598376 A GB 1598376A
- Authority
- GB
- United Kingdom
- Prior art keywords
- coal
- sodium hydroxide
- acid
- mixture
- liquefaction
- 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
- 239000003245 coal Substances 0.000 title claims description 75
- 238000000034 method Methods 0.000 title claims description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 84
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 25
- 150000001735 carboxylic acids Chemical class 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 6
- 235000011054 acetic acid Nutrition 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- -1 unsaturated aliphatic monocarboxylic acids Chemical class 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 150000007513 acids Chemical class 0.000 claims description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 4
- 230000000153 supplemental effect Effects 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002802 bituminous coal Substances 0.000 claims description 3
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 239000005711 Benzoic acid Substances 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- 239000001361 adipic acid Substances 0.000 claims description 2
- 235000011037 adipic acid Nutrition 0.000 claims description 2
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- 235000010233 benzoic acid Nutrition 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- 238000007796 conventional method Methods 0.000 claims description 2
- 239000000446 fuel Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 230000001737 promoting effect Effects 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000001384 succinic acid Substances 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 14
- 238000005470 impregnation Methods 0.000 description 2
- 239000003077 lignite Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L9/00—Treating solid fuels to improve their combustion
- C10L9/02—Treating solid fuels to improve their combustion by chemical means
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/04—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Solid Fuels And Fuel-Associated Substances (AREA)
Description
(54) A PROCESS FOR THE LIQUEFACTION OF COAL
(71) I, KUNITOSHI SHIMIZU, of
Japanese nationality, of No. 600, Kowata,
Chigasaki-shi, Kanagawa-Ken, Japan, do hereby declare the invention for which I pray that a Patent may be granted to me and the method by which it is to be performed to be particularly described in and by the following statement:
The present invention relates to a process of liquefaction of coal without employing high temperatures and pressures.
There are known processes for liquefying coal in which coal is decomposed under high temperature and high pressure. However, in such processes, very large amounts of energy are required to obtain a liquefied product, i.e. oil, useful as a source of energy and these processes are therefore not economically viable. Moreover, it is not possible to carry out the liquefaction of coal on a large scale using these processes.
It is an object of the present invention to provide a process for the liquefaction of coal, which does not require high temperature and high pressure.
Therefore according to the invention there is provided a process for the liquefaction of coal comprising the steps of:
i) impregnating granular coal with an aqueous solution of sodium hydroxide,
ii) drying the impregnated coal,
iii) pulverizing the treated coal to a particle size of less than 100 mesh,
iv) mixing the pulverized coal with an aqueous solution containing sodium hydroxide and an organic carboxylic acid and allowing the mixture to stand until signs of liquefaction appear and
v) adding water to the mixture and heating to a temperature of 90 to 1500C to form the liquefied product floating above the aqueous layer.
The liquefied product of coal obtained by the process according to the present invention comprises substances which are particularly useful as fuel oil and as starting materials for many chemical products.
Every sort of coal may be used in the process of the invention, for example, smokeless coal, bituminous coal, brown coal and lignite the term 'coal' used herein should be construed accordingly.
The granular coal used in the invention may be that supplied direct from conventional crushing machine and has a maximum average particle size of 3 cm, preferably about 2 cm.
The aqueous solution of caustic soda for impregnating the granular coal, is preferably a solution obtained by dissolving sodium hydroxide in demineralized water.
The concentration of the solution is generally in the range of from 1 to 5% by weight preferably 2 to 4% by weight, the most preferred concentration being about 3% by weight. It is preferred to use the solution in a 1:1 weight ratio with the granular coal.
The time, during which the granular coal is soaked with the solution to cause impregnation varies in accordance with the size of the granulated coal and the concentration of the solution. Generally the impregnation takes several hours, e.g. 10 hours or more.
The impregnated coal is dried, preferably as thoroughly as possible. Conventional drying apparatus may be used or the coal may be dried in the sun.
After drying the coal is pulverized, e.g. in a conventional pulverizer, to an average particle size smaller than 100 mesh (JIS A 1102) and preferably to a size of about 150 mesh.
The aqueous solution for treating the pulverized coal preferably contains sodium hydroxide and organic carboxylic acid in a molar ratio of from 0.5:1.5 to 1.5:0.5 and more preferably from 0.9:1.1 to 1.1:0.9. The sodium hydroxide and organic carboxylic acid form a sodium carboxylate salt and thus the aqueous solution consists of the salt together with any excess of sodium hydroxide or carboxylic acid. The total content of sodium hydroxide and organic carboxylic acid contained in the solution is preferably a maximum of about 10% by weight with respect to water. A total content of 4.5 to 6.0% by weight with respect to water is particularly preferred. The use of demineralized water is preferred as the solvent. The amount of the pulverized coal mixed with the solution of sodium hydroxide and carboxylic acid is preferably from 0.5 to 2 parts by weight per part by weight of the solution.
Suitable organic carboxylic acid for use in the invention are lower carboxylic acids containing up to 4 carbon atoms which are substantially liquid at normal temperature and exhibit boiling points lying in the range from 50 to 170 C, e.g. formic acid, acetic acid, propionic acid and butyric acid; saturated and unsaturated aliphatic monocarboxylic acids, e.g. acrylic acid and methacrylic acid; aliphatic polycarboxylic acids, e.g. malonic acid, succinic acid and adipic acid; and aromatic carboxylic acids, e.g.
benzoic acid. Formic acid and acetic acid are the preferred acids.
After the mixing of pulverized coal with the solution of sodium hydroxide and carboxylic acid the mixture is allowed to stand for the time required for the coal to be denatured and to show the first signs of liquefaction. Generally the time period is from about 5 to about 10 hours.
After the mixture shows signs of liquefaction, a supplemental amount of water preferably demineralized water is added, preferably in an amount from 0.3 to 1 parts by weight per part by weight of the pulverized coal. e coal mixture may optionally be transferred into a separate vessel, e.g. a kettle, for the subsequent heating treatment before or after the addition of water. After the supplemental addition of demineralized water, the mixture is heated to a temperature of from 90 to 1500C, preferably from 110 to 1200C. The duration of the heating depends on the temperature employed and generally is from about 30 minutes to about 2 hours.
After the heat treatment, up to about 80% of coal originally present is liquefied and floats above the aqueous layer. The separation of this liquefied product can easily be carried out by conventional methods.
It is possible to promote the liquefaction of coal, by adding an amount of phenol or naphthalene before the heating. These compounds may have a function of promoting the oxidation reaction during the liquefaction of coal.
The liquefied product of coal according to the present invention can either be used as such for fuel or subjected to fractioning into the constituent compounds.
The process of the liquefaction of coal according to the present invention has the advantages that it does not require high temperatures or high pressures and the apparatus employed is not complex. Furthermore, each step in the process is not complicated and the process can be carried out very economically and on a large scale.
The invention will now be illustrated by the following Example.
Example
A bituminous coal was crushed using a hammer crusher into particles having an average particle size of 2 cm. 10 kg of the granulated coal were introduced into a vessel having a capacity of 180t and containing an aqueous solution prepared by dissolving 300 g of sodium hydroxide in 10 kg of demineralized water. The resulting mixture was allowed to stand for 20 hours.
The impregnated coal was then removed and dried in the sun for 24 hours.
The dried impregnated coal was pulverized in a pulverizer to an average particle size of 150-mesh. 10 kg of this coal powder were introduced into an aqueous solution prepared by dissolving 300 g of sodium hydroxide and 400 g of acetic acid in 10 kg of demineralized water and the mixture is stirred to ensure thorough mixing. The mixture was then allowed to stand for 10 hours.
The resulting mixture was transferred into a kettle and, after the addition of 5 kg of demineralized water, the mixture was boiled for 1 hour at a temperature of 1200C. An oily product was obtained in the upper layer of the kettle amounting to 7.92 kg.
The yield of the liquefaction of the coal was calculated to be about 80%.
WHAT I CLAIM IS:
1. A process for the liquefaction of coal comprising the steps of:
i) impregnating granular coal with an aqueous solution of sodium hydroxide,
ii) drying the impregnated coal,
iii) pulverizing the treated coal to a particle size of less than 100 mesh,
iv) mixing the pulverized coal with an aqueous solution containing sodium hydroxide and an organic carboxylic acid and allowing the mixture to stand until signs of liquefaction appear and
v) adding water to the mixture and heating to a temperature of 90 to 1500C to form the liquefied product floating above the aqueous layer.
2. A process as claimed in Claim 1 wherein the average particle size of the granulated coal is a maximum of 3 cm.
3. A process as claimed in Claim 1 or
Claim 2 in which the average particle size of the pulverized coal is about 150-mesh.
**WARNING** end of DESC field may overlap start of CLMS **.
Claims (14)
1. A process for the liquefaction of coal comprising the steps of:
i) impregnating granular coal with an aqueous solution of sodium hydroxide,
ii) drying the impregnated coal,
iii) pulverizing the treated coal to a particle size of less than 100 mesh,
iv) mixing the pulverized coal with an aqueous solution containing sodium hydroxide and an organic carboxylic acid and allowing the mixture to stand until signs of liquefaction appear and
v) adding water to the mixture and heating to a temperature of 90 to 1500C to form the liquefied product floating above the aqueous layer.
2. A process as claimed in Claim 1 wherein the average particle size of the granulated coal is a maximum of 3 cm.
3. A process as claimed in Claim 1 or
Claim 2 in which the average particle size of the pulverized coal is about 150-mesh.
4. A process as claimed in any preceding
claim in which the concentration of the aqueous solution of sodium hydroxide for impregnating the granulated coal is in the range of from 1 to 5% by weight.
5. A process as claimed in Claim 4 in which the concentration of the aqueous solution of sodium hydroxide is from 2 to 4% by weight.
6. A process as claimed in Claim 5 in which the concentration of the aqueous solution of sodium hydroxide is about 3% by weight.
7. A process as claimed in any preceding claim in which the molar ratio of sodium hydroxide to organic carboxylic acid in the aqueous solution for treating the pulverized coal is from 0.5:1.5 to 1.5:0.5.
8. A process as claimed in Claim 7 in which the molar ratio of sodium hydroxide to organic carboxylic acid is from 0.9:1.1 to 1.1:0.9.
9. A process as claimed in any preceding claim in which the total content of sodium hydroxide and organic carboxylic acid in the solution for treating the pulverized coal is a maximum of 10% by weight with respect to the water.
10. A process as claimed in any preceding claim in which the organic carboxylic acid is a lower carboxylic acid containing up to 4 carbon atoms.
11. A process as claimed in any preced- ing claim in which the amount of the water added in step v) is from 0.3 to 1 part by weight per one part by weight of the pulverized coal.
12. A process as claimed in any preceding claim in which phenol or naphthalene is additionally added before heating the pulverized coal mixture.
13. A process for the liquefaction of coal substantially as herein described with reference to the Example.
14. The liquefied product obtained from a process as claimed in any preceding claim.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2286077A JPS53108106A (en) | 1977-03-04 | 1977-03-04 | Liquefaction of coal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB1598376A true GB1598376A (en) | 1981-09-16 |
Family
ID=12094460
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB8579/78A Expired GB1598376A (en) | 1977-03-04 | 1978-03-03 | Process for the liquefaction of coal |
Country Status (11)
| Country | Link |
|---|---|
| JP (1) | JPS53108106A (en) |
| AU (1) | AU506275B1 (en) |
| BE (1) | BE864544A (en) |
| BR (1) | BR7801321A (en) |
| CA (1) | CA1104960A (en) |
| DE (1) | DE2808670C3 (en) |
| DK (1) | DK153086C (en) |
| FR (1) | FR2382492A1 (en) |
| GB (1) | GB1598376A (en) |
| IT (1) | IT1105882B (en) |
| NL (1) | NL185526C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1981000720A1 (en) * | 1979-09-11 | 1981-03-19 | K Shimizu | Process for liquefying coal |
| FR2464985A1 (en) * | 1979-09-12 | 1981-03-20 | Kunitoshi Shimizu | Oil prodn. by liquefaction of coal - by agitation with aq. alkali |
| GB2236323B (en) * | 1989-09-28 | 1993-07-21 | Nat Energy Council | Coal solubilisation |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE302397C (en) * | ||||
| US1608075A (en) * | 1920-08-26 | 1926-11-23 | Wallin Johan Hugo | Process of destructive decomposition of organic substances |
| DE640522C (en) * | 1930-12-24 | 1937-01-06 | Wilhelm R Roederer Dr | Process for the extraction of bitumen from bituminous lignite |
| GB446494A (en) * | 1934-07-28 | 1936-04-28 | Charles Vieu | Improvements in or relating to the treatment of coal and other solid carbonaceous materials for use in subsequent hydrogenation processes |
| FR2311086A1 (en) * | 1975-05-12 | 1976-12-10 | Battelle Memorial Institute | Coal and coke treatment with aq (bi)carbonate - which removes sulphur and toxi ash components |
-
1977
- 1977-03-04 JP JP2286077A patent/JPS53108106A/en active Granted
-
1978
- 1978-03-01 DE DE2808670A patent/DE2808670C3/en not_active Expired
- 1978-03-01 CA CA298,020A patent/CA1104960A/en not_active Expired
- 1978-03-02 AU AU33759/78A patent/AU506275B1/en not_active Expired
- 1978-03-02 DK DK094078A patent/DK153086C/en active
- 1978-03-03 NL NLAANVRAGE7802386,A patent/NL185526C/en not_active IP Right Cessation
- 1978-03-03 IT IT03350/78A patent/IT1105882B/en active
- 1978-03-03 GB GB8579/78A patent/GB1598376A/en not_active Expired
- 1978-03-03 FR FR7806112A patent/FR2382492A1/en active Granted
- 1978-03-03 BR BR7801321A patent/BR7801321A/en unknown
- 1978-03-03 BE BE185655A patent/BE864544A/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5415564B2 (en) | 1979-06-15 |
| FR2382492A1 (en) | 1978-09-29 |
| NL7802386A (en) | 1978-09-06 |
| NL185526B (en) | 1989-12-01 |
| BE864544A (en) | 1978-07-03 |
| DK94078A (en) | 1978-09-05 |
| DK153086B (en) | 1988-06-13 |
| IT7803350A0 (en) | 1978-03-03 |
| NL185526C (en) | 1990-05-01 |
| AU506275B1 (en) | 1979-12-20 |
| DK153086C (en) | 1988-11-07 |
| DE2808670C3 (en) | 1981-06-04 |
| DE2808670B2 (en) | 1980-07-17 |
| JPS53108106A (en) | 1978-09-20 |
| DE2808670A1 (en) | 1978-09-07 |
| IT1105882B (en) | 1985-11-04 |
| BR7801321A (en) | 1978-09-26 |
| FR2382492B1 (en) | 1984-06-08 |
| CA1104960A (en) | 1981-07-14 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PS | Patent sealed [section 19, patents act 1949] | ||
| PCNP | Patent ceased through non-payment of renewal fee |