GB2290291A - Methanol purification - Google Patents
Methanol purification Download PDFInfo
- Publication number
- GB2290291A GB2290291A GB9411311A GB9411311A GB2290291A GB 2290291 A GB2290291 A GB 2290291A GB 9411311 A GB9411311 A GB 9411311A GB 9411311 A GB9411311 A GB 9411311A GB 2290291 A GB2290291 A GB 2290291A
- Authority
- GB
- United Kingdom
- Prior art keywords
- mixture
- methanol
- heated
- base
- purified
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Feedstock Methanol containing impurities such as Acetone, Methyl Ethyl Ketone, Water, Formic Acid, Formaldehyde, Acetic Acid and Methyl Esters is purified by adding the feedstock together with a reducing agent such as lithium aluminium hydride to the reflux vessel of a batch distillation unit. The mixture is heated for at least half an hour at a temperature of at least 65 DEG C. A strong base such as potassium hydroxide is then added and the mixture is heated to reflux. The optional final stage in the purification process involves adding a weak base such as sodium carbonate and heating the mixture under reflux. A very high level of purity of at least 99.9% is obtained.
Description
"Solvent Purification"
The invention relates to solvent purification, in particular to a process for purifying Methanol containing impurities such as Acetone, Methyl Ethyl Ketone, Water,
Formic Acid, Formaldehyde, Acetic Acid and Methyl Esters, catalytic amounts of acid and the like.
Methanol is widely used in selective recrystallisation and extractive distillation. Because of its favourable dielectric, solvent and optical properties it is also widely used in analytical chemistry, particularly in high performance liquid chromatography (hplc), organic synthesis, pesticide residue analysis, W and IR spectroscopy, purge and trap analysis, and DNA and peptide synthesis.
As analytical chemistry techniques and analytical machines become ever more sophisticated there is a need to develop processes for producing Methanol to a very high level of purity for use as a standard in such equipment.
This invention is therefore directed towards providing a process for producing Methanol having a very high level of purity in a cost efficient manner.
According to the invention there is provided a purification process for the purification of Methanol containing impurities such as Acetone, Methyl Ethyl
Ketone, Water, Formic Acid, Formaldehyde, Acetic Acid and
Methyl Esters to produce highly purified Methanol, the process comprising of the steps of :
adding a reducing agent to Methanol containing said
impurities;
adding a strong base to the mixture;
distilling the mixture in a distillation column; and
recovering purified Methanol from the distillation
column.
In one particularly preferred embodiment of the invention the Methanol is further purified by adding an additional base to the mixture prior to distillation. Preferably, the additional base is a weak base such as sodium carbonate.
Preferably the mixture is heated after addition of the reducing agent. Advantageously the mixture is heated to a temperature of at least 650C for a period of one hour.
In a preferred embodiment of the invention, after addition of the base, the mixture is heated to reflux and the mixture is sampled over time to monitor the levels of impurities present.
In one embodiment of the invention the mixture is cooled prior to addition of the base.
Preferably, the reducing agent is lithium aluminium hydride.
The invention also provides purified Methanol whenever purified by the process of the invention.
The invention will be more clearly understood from the following description thereof given by way of example only with reference to the accompanying drawing which is a schematic diagram of a custom designed distillation apparatus used in the process of the invention.
Referring to the drawing, there is illustrated a custom designed distillation apparatus used in the process of the invention comprising a distillation column 1 of packed raschig rings having from 30 to 40 theoretical plates.
Feed material is added into a boiling vessel 2 through an inlet valve 3. The feed material is heated by passing through a reboiler 5 having a steam heated coil 6. Vapour from the distillation column 1 is condensed by passing cooling water through a coil 7 in the condenser 8. Reflux material is returned to the column 1 through a reflux line 9. When the desired purity level has been reached the material is fed through an outlet line 10 to a collection vessel 12. The material may be passed through molecular sieves 11 prior to delivery to the collection vessel 12.
EXAMPLE
Feedstock Methanol containing impurities such as Acetone,
Methyl Ethyl Ketone, Water, Formic Acid, Formaldehyde,
Acetic Acid and Methyl Esters was purified by the following process.
100L of feedstock Methanol is added to the reflux vessel described above and approximately SOg of a reducing agent such as lithium aluminium hydride is added. A small quantity of a strong base such as potassium hydroxide is also added. The strong base acts as an hydrolysing agent.
The mixture is then heated for at least one hour at a temperature of at least 65"C. A weak base such as sodium carbonate is then added to the mixture in an amount of at least 100g (up to 500g) and the mixture is heated to reflux. The levels of impurity present are monitored.
When the levels of impurities have reached desired values the mixture is allowed to cool.
The Methanol purified by this process has a purity of at least 99.9% with a water content of less than 0.1%, an acidity level of less than .001% and a residue level of less than .0001%.
The high grade purified Methanol is used in HPLC analysis and has a wide range of application including applications in organic synthesis and in residue analyses, purge and trap analysis and UV-IR Spectroscopy.
The invention is not limited to the embodiment hereinbefore described which may be varied in detail.
Claims (11)
1. A purification process for the purification of
Methanol containing impurities such as Acetone,
Methyl Ethyl Ketane, Water, Formic Acid,
Formaldehyde, Acetic Acid and Methyl Esters to
produce Methanol, the process comprising the steps
of :
adding a reducing agent to Methanol
containing impurities;
adding a strong base to the mixture;
distilling the mixture in a distillation
column; and
recovering purified Methanol from the
distillation column.
2. A process as claimed in claim 1 wherein the strong
base is potassium hydroxide.
3. A process as claimed in claim 1 or 2 wherein the
Methanol is further purified by adding an
additional base to the mixture prior to
distillation.
4. A process as claimed in claim 3 wherein the
additional base is a weak base.
5. A process as claimed in claim 4 wherein the
additional base is sodium carbonate.
6. A process as claimed in any of claims 1 to 5
wherein the mixture is heated after addition of
the reducing agent.
7. A process as claimed in claim 6 wherein the
mixture is heated to a temperature of at least 650C
for a period of at least one hour.
8. A process as claimed in any of claims 2 to 7
wherein, after addition of the base, the mixture
is heated to reflux and the mixture is sampled
over time to monitor the levels of impurities
present.
9. A process as claimed in any preceding claim
wherein the reducing agent is lithium aluminium
hydride.
10. A process substantially as hereinbefore described
with reference to the Examples.
11. Purified Methanol whenever purified by a process
as claimed in any preceding claim.
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB9411311A GB2290291B (en) | 1994-06-07 | 1994-06-07 | Methanol purification |
BE9400597A BE1006528A6 (en) | 1994-06-07 | 1994-06-23 | Purification solvent. |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB9411311A GB2290291B (en) | 1994-06-07 | 1994-06-07 | Methanol purification |
BE9400597A BE1006528A6 (en) | 1994-06-07 | 1994-06-23 | Purification solvent. |
Publications (3)
Publication Number | Publication Date |
---|---|
GB9411311D0 GB9411311D0 (en) | 1994-07-27 |
GB2290291A true GB2290291A (en) | 1995-12-20 |
GB2290291B GB2290291B (en) | 1998-05-13 |
Family
ID=25662889
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
GB9411311A Expired - Fee Related GB2290291B (en) | 1994-06-07 | 1994-06-07 | Methanol purification |
Country Status (2)
Country | Link |
---|---|
BE (1) | BE1006528A6 (en) |
GB (1) | GB2290291B (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB2322812A (en) * | 1997-03-03 | 1998-09-09 | G K Analytical Sciences Limite | Solvent purification |
WO2004072007A1 (en) * | 2003-02-06 | 2004-08-26 | Honeywell International Inc. | Purification of alcohol |
CN105541553A (en) * | 2016-02-23 | 2016-05-04 | 衡阳市凯信化工试剂股份有限公司 | Preparation and purification method and device of high performance liquid chromatography (HPLC) solvent |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB344796A (en) * | 1929-12-10 | 1931-03-10 | James Ritchie Park | Improved method for the purification of synthetic alcohols |
GB659727A (en) * | 1948-11-19 | 1951-10-24 | Celanese Corp | Process for the recovery of methylol, methanol and alkali metal formates |
GB1520709A (en) * | 1977-05-20 | 1978-08-09 | Inst Neftechimicheskogo Sintez | Process for producing c3 - c20 aliphatic alcohols |
-
1994
- 1994-06-07 GB GB9411311A patent/GB2290291B/en not_active Expired - Fee Related
- 1994-06-23 BE BE9400597A patent/BE1006528A6/en not_active IP Right Cessation
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB344796A (en) * | 1929-12-10 | 1931-03-10 | James Ritchie Park | Improved method for the purification of synthetic alcohols |
GB659727A (en) * | 1948-11-19 | 1951-10-24 | Celanese Corp | Process for the recovery of methylol, methanol and alkali metal formates |
GB1520709A (en) * | 1977-05-20 | 1978-08-09 | Inst Neftechimicheskogo Sintez | Process for producing c3 - c20 aliphatic alcohols |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB2322812A (en) * | 1997-03-03 | 1998-09-09 | G K Analytical Sciences Limite | Solvent purification |
GB2322812B (en) * | 1997-03-03 | 2001-03-14 | G K Analytical Sciences Ltd | Solvent purification |
WO2004072007A1 (en) * | 2003-02-06 | 2004-08-26 | Honeywell International Inc. | Purification of alcohol |
CN105541553A (en) * | 2016-02-23 | 2016-05-04 | 衡阳市凯信化工试剂股份有限公司 | Preparation and purification method and device of high performance liquid chromatography (HPLC) solvent |
CN105541553B (en) * | 2016-02-23 | 2018-09-28 | 衡阳市凯信化工试剂股份有限公司 | A kind of high-efficient liquid phase chromatogram HPLC solvent prepares purification process and device |
Also Published As
Publication number | Publication date |
---|---|
BE1006528A6 (en) | 1994-10-04 |
GB9411311D0 (en) | 1994-07-27 |
GB2290291B (en) | 1998-05-13 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
PCNP | Patent ceased through non-payment of renewal fee |
Effective date: 20100607 |