CN108586228A - A kind of preparation method of formic acid - Google Patents
A kind of preparation method of formic acid Download PDFInfo
- Publication number
- CN108586228A CN108586228A CN201810583641.2A CN201810583641A CN108586228A CN 108586228 A CN108586228 A CN 108586228A CN 201810583641 A CN201810583641 A CN 201810583641A CN 108586228 A CN108586228 A CN 108586228A
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- solution
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- formic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/10—Preparation of carboxylic acids or their salts, halides or anhydrides by reaction with carbon monoxide
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention is a kind of preparation method of formic acid, and raw materials used is NaOH, CO, and this method is formed through high-pressure synthesis, acid tune, crystallization, recrystallization, washing, drying；It comprises the concrete steps that the NaOH solution for first preparing saturation is put into high-pressure reactor, CO gases is injected into reactor；Then reactor is down to normal temperature and pressure, adjusts pH value；It is diluted with water solution, then reactor is placed in mixture of ice and water, solution is down to 16 DEG C, is stood；Crystal is filtered, is re-dissolved with hot water, is then replaced in mixture of ice and water, solution is down to 16 DEG C, is stood；It is washed with absolute ethyl alcohol；Finally formic acid obtained is dried with anhydrous calcium chloride.The method of the present invention concise in technology, final products are single, and no other byproducts generate, product purity and high income.
Description
Technical field
The present invention relates to a kind of production methods of Organic Chemicals, and in particular to a kind of preparation method of formic acid.
Background technology
Formic acid is one of basic organic chemical industry raw material, and it is industrial to be widely used in pesticide, leather, dyestuff, medicine and rubber etc., also serves as
Disinfectant and preservative.Formic acid can be directly used for fabric processing, tanning, the storage of fabrics printing and dyeing and greenfeed, it is also possible to make
Metal conditioner, rubber chemicals and industrial solvent.In organic synthesis for synthesize various formic acid esters, acridine dye and
Carboxamide series medicine intermediate.
Traditional formic acid production is mainly reacted using methanol and CO in the presence of catalyst sodium methoxide, generates methyl formate, then
Again formic acid and methanol are generated through hydrolysis.Methanol is recyclable to be sent into methyl formate reactor, and formic acid can be obtained difference through rectifying again
The product of specification.
Invention content
The technical problem to be solved by the present invention is in view of the deficiencies of the prior art, provide a kind of new, method reasonable design, can
The formic acid preparation method of strong operability.
The technical problem to be solved by the present invention is to what is realized by technical solution below.The present invention is a kind of system of formic acid
Preparation Method, its main feature is that：Raw materials used is NaOH, CO, and this method is through high-pressure synthesis, sour tune, crystallization, recrystallization, washing, drying
It forms；The NaOH solution for preparing saturation is put into high-pressure reactor, under conditions of 170-190 DEG C, 2-3MPa, to reactor
Interior injection CO gases, until solution ph is 6.5-7.5；Reactor is down to normal temperature and pressure, is 20-30% with mass concentration
Hydrochloride adjusted solution pH value be 1-2；Then the water that solution monoploid product is added is set reactor with the concentration of dilute solution
In mixture of ice and water, solution is down to 1-6 DEG C, stands 20 hours；Crystal is filtered, it is again molten with 80-85 DEG C of hot water
Solution, is then replaced in mixture of ice and water, and solution is down to 1-6 DEG C, stands 20 hours；It is washed 1-3 times with absolute ethyl alcohol；
Formic acid obtained is dried with anhydrous calcium chloride.
The preparation method of formic acid of the present invention, further：The NaOH solution for preparing saturation is put into high-pressure reactor,
180 DEG C, under conditions of 2.5MPa, CO gases are injected into reactor, until solution ph is 7.
The preparation method of formic acid of the present invention, further：Reactor is down to normal temperature and pressure, is 25% with mass concentration
Hydrochloride adjusted solution pH value be 1.5.
The preparation method of formic acid of the present invention, further：The water of solution monoploid product is added, with dilute solution
Then reactor is placed in mixture of ice and water by concentration, solution is down to 3 DEG C, stands 20 hours.
The preparation method of formic acid of the present invention, further：Crystal is filtered, is re-dissolved with 82 DEG C of hot water, so
After be replaced in mixture of ice and water, solution is down to 3 DEG C, stands 20 hours；It is washed 2 times with absolute ethyl alcohol.
Compared with prior art, present invention process is succinct, and final products are single, and no other byproducts generate, product purity and receipts
Rate is high.
Specific implementation method
The specific technical solution of the present invention described further below, in order to which those skilled in the art is further understood that this hair
It is bright, without constituting the limitation to its right.
Embodiment 1, a kind of preparation method of formic acid, it is raw materials used be NaOH, CO, this method through high-pressure synthesis, acid adjust, crystallization,
Recrystallization, washing, drying form；The NaOH solution for preparing saturation is put into high-pressure reactor, in 170-190 DEG C, 2-3MPa
Under conditions of, CO gases are injected into reactor, until solution ph is 6.5-7.5；Reactor is down to normal temperature and pressure, uses matter
The hydrochloride adjusted solution pH value for measuring a concentration of 20-30% is 1-2；The water of solution monoploid product is added, with the dense of dilute solution
Reactor, is then placed in mixture of ice and water by degree, and solution is down to 1-6 DEG C, stands 20 hours；Crystal is filtered, 80- is used
85 DEG C of hot water re-dissolves, and is then replaced in mixture of ice and water, and solution is down to 1-6 DEG C, stands 20 hours；With anhydrous
Ethyl alcohol washs 1-3 times；Formic acid obtained is dried with anhydrous calcium chloride.
Embodiment 2, in the preparation method of formic acid described in embodiment 1：The NaOH solution for preparing saturation is put into high-pressure reactor,
Under conditions of 180 DEG C, 2.5MPa, CO gases are injected into reactor, until solution ph is 7.
Embodiment 3, in the preparation method of formic acid described in embodiment 1：Reactor is down to normal temperature and pressure, is with mass concentration
25% hydrochloride adjusted solution pH value is 1.5.
Embodiment 4, in the preparation method of formic acid described in embodiment 1：The water of solution monoploid product is added, with the dense of dilute solution
Reactor, is then placed in mixture of ice and water by degree, and solution is down to 3 DEG C, stands 20 hours.
Embodiment 5, in the preparation method of formic acid described in embodiment 1：Crystal is filtered, is re-dissolved with 82 DEG C of hot water,
Then it is replaced in mixture of ice and water, solution is down to 3 DEG C, stands 20 hours；It is washed 2 times with absolute ethyl alcohol.
Claims (5)
1. a kind of preparation method of formic acid, it is characterised in that：It is raw materials used be NaOH, CO, this method through high-pressure synthesis, acid adjust,
Crystallization, recrystallization, washing, drying form；The NaOH solution for preparing saturation is put into high-pressure reactor, in 170-190 DEG C, 2-
Under conditions of 3MPa, CO gases are injected into reactor, until solution ph is 6.5-7.5；Reactor is down to normal temperature and pressure,
The hydrochloride adjusted solution pH value for being 20-30% with mass concentration is 1-2；The water of solution monoploid product is added, with dilute solution
Then reactor is placed in mixture of ice and water by concentration, solution is down to 1-6 DEG C, stands 20 hours；Crystal is filtered, is used
80-85 DEG C of hot water re-dissolves, and is then replaced in mixture of ice and water, and solution is down to 1-6 DEG C, stands 20 hours；With
Absolute ethyl alcohol washs 1-3 times；Formic acid obtained is dried with anhydrous calcium chloride.
2. the preparation method of formic acid according to claim 1, it is characterised in that：The NaOH solution for preparing saturation is put into high pressure
In reactor, under conditions of 180 DEG C, 2.5MPa, CO gases are injected into reactor, until solution ph is 7.
3. the preparation method of formic acid according to claim 1, it is characterised in that：Reactor is down to normal temperature and pressure, uses matter
The hydrochloride adjusted solution pH value for measuring a concentration of 25% is 1.5.
4. the preparation method of formic acid according to claim 1, it is characterised in that：The water of solution monoploid product is added, with dilute
Reactor, is then placed in mixture of ice and water by the concentration for releasing solution, and solution is down to 3 DEG C, stands 20 hours.
5. the preparation method of formic acid according to claim 1, it is characterised in that：Crystal is filtered, with 82 DEG C of hot water
It re-dissolves, is then replaced in mixture of ice and water, solution is down to 3 DEG C, stands 20 hours；It is washed 2 times with absolute ethyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810583641.2A CN108586228A (en) | 2018-06-08 | 2018-06-08 | A kind of preparation method of formic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810583641.2A CN108586228A (en) | 2018-06-08 | 2018-06-08 | A kind of preparation method of formic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108586228A true CN108586228A (en) | 2018-09-28 |
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ID=63623245
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810583641.2A Withdrawn CN108586228A (en) | 2018-06-08 | 2018-06-08 | A kind of preparation method of formic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108586228A (en) |
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2018
- 2018-06-08 CN CN201810583641.2A patent/CN108586228A/en not_active Withdrawn
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Application publication date: 20180928 |