CN203683423U - Preparation device used for formic acid - Google Patents
Preparation device used for formic acid Download PDFInfo
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- CN203683423U CN203683423U CN201320530511.5U CN201320530511U CN203683423U CN 203683423 U CN203683423 U CN 203683423U CN 201320530511 U CN201320530511 U CN 201320530511U CN 203683423 U CN203683423 U CN 203683423U
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- rectifying tower
- communicated
- formic acid
- input aperture
- delivery port
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Abstract
The utility model discloses a preparation device used for formic acid. The preparation device comprises a preparation device body used for formic acid, which is provided with a pre-mixer (3), a hydrolysis reactor (6), a rectifying tower I (7) and a rectifying tower II (12), wherein the pre-mixer (3) is used for mixing hydrated methyl formate; the hydrolysis reactor (6) is communicated with the pre-mixer (3); the rectifying tower I (7) is communicated with the hydrolysis reactor (6); the rectifying tower II (12) is communicated with the rectifying tower I (7); a top-end output port end of the rectifying tower II (12) is set to be communicated with an input port end of the pre-mixer (3); by-products in a secondary rectifying tower separating process are used as a catalyst for hydrolysis reaction of the hydrated methyl formate, so that the catalyst is not needed to be externally added and other side reactions do not occur, and therefore, quality of the formic acid is improved.
Description
One, technical field
The utility model relates to a kind of device for making for formic acid, especially a kind of preparation method of the formic acid with two stage rectification tower and device.
Two, background technology
Formic acid is one of basic organic chemical industry raw material, be widely used in agricultural chemicals, leather, dyestuff, the industry such as medicine and rubber, formic acid can be directly used in fabric processing, tanning, the storage of fabrics printing and dyeing and green fodder, also can be used as metal conditioner, rubber ingredients and industrial solvent, in organic synthesis for the synthesis of various manthanoate, acridine dye and methane amide series medicine intermediate, therefore formic acid is a kind of important Chemicals, at the existing device for making for formic acid, need additional mineral acid catalysis, make hydrolysis conversion very low because there is reverse esterification simultaneously.
Three, summary of the invention
In order to overcome above-mentioned technical disadvantages, the purpose of this utility model is to provide a kind of device for making for formic acid, has therefore improved the quality of formic acid.
For achieving the above object, the technical scheme that the utility model is taked is: include there is premixer, the device for making body of the formic acid of hydrolysis reactor, rectifying tower I and rectifying tower II, wherein, for water and the mixed premixer of methyl-formiate, the hydrolysis reactor being communicated with premixer, the rectifying tower I being communicated with hydrolysis reactor, the rectifying tower II that is communicated with rectifying tower I, the top delivery port end of rectifying tower II is set to be communicated with the input aperture end of premixer.
Owing to having designed the by-product of two-stage rectification tower sepn process as the catalyzer of water and methyl formate hydrolysis reaction, do not need extra catalyst, there is not other side reaction yet, therefore improve the quality of formic acid.
The utility model has designed, the device for making body of formic acid also includes preheater, reboiler I, condenser I, reboiler II and condenser II, the input aperture end of premixer is set to be communicated with water pot and methyl-formiate tank respectively, premixer delivery port end is set to be communicated with the input aperture end of hydrolysis reactor by preheater, hydrolysis reactor delivery port end is set to be communicated with the input aperture end of rectifying tower I, reboiler I is set to be communicated with the heating source of rectifying tower I, the top gas delivery port end of rectifying tower I is set to be communicated with the input aperture end of condenser I, the delivery port end of condenser I is set to a road and is communicated with the input aperture end of rectifying tower I, another road is communicated with the input aperture end of methyl-formiate synthetic tower, the bottom delivery port end of rectifying tower I is set to be communicated with the input aperture end of rectifying tower II by the pump housing, reboiler II is set to be communicated with the heating source of rectifying tower II, the top gas delivery port end of rectifying tower II is set to be communicated with the input aperture end of condenser II, the delivery port end of condenser II is set to a road and is communicated with the input aperture end of rectifying tower II, another road is communicated with the input aperture end of premixer, the bottom delivery port end of rectifying tower II is set to be communicated with the input aperture end of formic acid finished pot by the pump housing.
The utility model has designed, and rectifying tower I is set to one-level rectifying tower, and rectifying tower II is set to two-stage rectification tower.
The utility model has designed, and also includes flash distillation plant, and flash distillation plant is arranged in rectifying tower I.
The utility model has designed, flash distillation plant is set to include tank body, spray header and wire packing layer, on the top end face of tank body, be provided with gaseous phase outlet and be provided with liquid-phase outlet on the bottom face of tank body, spray header is arranged on the middle part of tank body 81, wire packing layer is arranged on the gaseous phase outlet position of tank body, and spray header is set to be communicated with hydrolysis reactor delivery port end.
In the technical program, premixer, hydrolysis reactor, rectifying tower I and rectifying tower II are important technology feature of the present utility model, in the technical field of the device for making for formic acid, there is novelty, creativeness and practicality, and in rectifying tower I, be provided with flash distillation plant, produce and improved the quality of formic acid and energy-conservation technique effect.
Four, brief description of the drawings
Fig. 1 is schematic diagram of the present utility model:
Fig. 2 is the schematic diagram of flash distillation plant 8.
Five, embodiment
Fig. 1 is an embodiment of the present utility model, illustrate by reference to the accompanying drawings the present embodiment, a kind of device for making for formic acid, include premixer 3, preheater 5, hydrolysis reactor 6, rectifying tower I 7, reboiler I 9, condenser I 10, rectifying tower II 12, reboiler II 14, condenser II 15 and flash distillation plant 8, flash distillation plant 8 is arranged in rectifying tower I 7, the input aperture end of premixer 3 is set to be communicated with water pot and methyl-formiate tank respectively, premixer 3 delivery port ends are set to be communicated with the input aperture end of hydrolysis reactor 6 by preheater 5, hydrolysis reactor 6 delivery port ends are set to be communicated with the input aperture end of rectifying tower I 7, reboiler I 9 is set to be communicated with the heating source of rectifying tower I 7, the top gas delivery port end of rectifying tower I 7 is set to be communicated with the input aperture end of condenser I 10, the delivery port end of condenser I 10 is set to a road and is communicated with the input aperture end of rectifying tower I 7, another road is communicated with the input aperture end of methyl-formiate synthetic tower, the bottom delivery port end of rectifying tower I 7 is set to be communicated with the input aperture end of rectifying tower II 12 by the pump housing, reboiler II 14 is set to be communicated with the heating source of rectifying tower II 12, the top gas delivery port end of rectifying tower II 12 is set to be communicated with the input aperture end of condenser II 15, the delivery port end of condenser II 15 is set to a road and is communicated with the input aperture end of rectifying tower II 12, another road is communicated with the input aperture end of premixer 3, the bottom delivery port end of rectifying tower II 12 is set to be communicated with the input aperture end of formic acid finished pot by the pump housing.
In the present embodiment, rectifying tower I 7 is set to one-level rectifying tower, and rectifying tower II 12 is set to two-stage rectification tower.
In the present embodiment, flash distillation plant 8 is set to include tank body 81, spray header 82 and wire packing layer 83, on the top end face of tank body 81, be provided with gaseous phase outlet and be provided with liquid-phase outlet on the bottom face of tank body 81, spray header 82 is arranged on the middle part of tank body 81, wire packing layer 83 is arranged on the gaseous phase outlet position of tank body 81, and spray header 82 is set to be communicated with hydrolysis reactor 6 delivery port ends.
Preparation method, while the steps include: that a water and methyl-formiate mix, adding content is the formic acid solution of 3-7%, then pass through successively hydrolysis reaction, the sepn process of one-level rectifying tower and the sepn process of two-stage rectification tower, the formic acid solution that wherein content is 3-7% is set to the by-product of two-stage rectification tower sepn process.
Concrete step is:
A, according to part by weight, water and methyl-formiate 1:1.4-1.7 are mixed, in the time mixing, adding content is the formic acid solution of 3-7%, forms binary liquid mixture.
B, be under 135-140 DEG C, the pressure environment that is 1.2-1.3Mpa in temperature, the binary liquid mixture reaction that is hydrolyzed.
The binary liquid mixture of c, process hydrolysis reaction enters in one-level rectifying tower, in temperature is the one-level rectifying tower of 95-105 DEG C, acts on and separating, entered condensation rear portion through the gas at the top of one-level rectifying tower and enter the mixture that one-level rectifying tower, another part enter the bottom of methyl-formiate synthetic tower, one-level rectifying tower and enter in two-stage rectification tower.
D, the mixture separating through one-level rectifying tower enter in two-stage rectification tower, in temperature is the one-level rectifying tower of 145-155 DEG C, separate, entered condensation rear portion through the gas at the top of two-stage rectification tower and enter two-stage rectification tower, another part to be content be that the formic acid solution of 3-7% mixes with water and the methyl-formiate mixed solution of the first step, the liquid of the bottom of two-stage rectification tower is the formic acid that content is 85%-95% again.
The formic acid solution of the lower concentration obtaining in rectifying tower II 12 top gases, is re-used as the catalyzer that water and methyl formate hydrolysis react, and does not need extra catalyst.Under flash distillation plant 8 effect, in rectifying tower I 7, methyl alcohol and methyl-formiate are flashed off rapidly, rise to tower top, at the bottom of formic acid and water are shifted to tower, and the one, effectively reduce duration of contact of formic acid and methyl alcohol; The 2nd, act on by flash distillation plant 8, rectifying tower I 7 feed separation are temperature required, pressure decreased, thereby suppress the resterification reaction of formic acid and methyl alcohol, adopt the utility model can make reverse esterification yield be controlled in 2%, one way hydrolysis conversion can reach 40%, is better than traditional technology because there is the level of reverse esterification hydrolysis conversion less than 20%; By reducing rectifying tower I 7 interior temperature, pressures, equipment and steam consumption have been reduced simultaneously.
The test of use the present embodiment, the formic acid of producing by the present embodiment, the aqueous formic acid returning by two towers is as autocatalysis agent, and without extra catalyst, there are not other side reactions in hydrolytic process, has broken away from the defect of in the past bringing with additional mineral acid catalysis.After hydrolysis, mixture, through reactor outlet pressure valve, enters the special flash distillation plant of a tower after decompression, and methyl alcohol and methyl-formiate are flashed off rapidly, rise to tower top, at the bottom of formic acid and water are shifted to tower.The one, effectively reduce duration of contact of formic acid and methyl alcohol; The 2nd,, pressure decreased temperature required by flash distillation plant one tower feed separation, thereby the reaction of the resterification of inhibition formic acid and methyl alcohol.Adopt the utility model can make reverse esterification yield be controlled in 2%, one way hydrolysis conversion can reach 40%, is better than traditional technology because there is the level of reverse esterification hydrolysis conversion less than 20%.Equipment and steam consumption have been reduced by reducing temperature, pressure in rectifying tower simultaneously.In industrial production, have the realistic problems such as per pass conversion is low, operational requirement is high now, existing technique can improve per pass conversion and reduce energy consumption.The utility model is easy to operate, and reactor batching is easy to carry out serialization scale operation after mixing according to a certain percentage.
In the present embodiment, flash distillation plant 8 is divided into tank body 81 inner chambers the flash chamber that is positioned at the spray separate chamber of below and is positioned at top.The material inlet of flash distillation plant 8 is provided with spray equipment, the gas-liquid mixed material that enters flash distillation plant 8 carries out flash distillation after spray equipment spray, strengthen the flash distillation effect of gas-liquid mixed material, and further pass through the separation of wire packing, improve gas-liquid separation effect, improved the purity of isolated gas, liquid product.
The utlity model has lower feature:
1, because the by-product that has designed the sepn process of two-stage rectification tower is as the catalyzer of water and methyl formate hydrolysis reaction, do not need extra catalyst, there is not other side reaction yet, therefore improved the quality of formic acid.
2, owing to having designed the device that plays flash distillation effect, reduce the duration of contact of formic acid and methyl alcohol, improved the quality of formic acid, reduced the pressure and temperature of rectifying separation, reduced energy consumption.
3, owing to having designed premixer 3, preheater 5, hydrolysis reactor 6, rectifying tower I 7, reboiler I 9, condenser I 10, rectifying tower II 12, reboiler II 14 and condenser II 15, be applicable to large-scale formic acid and produce, improve day output.
Above-described embodiment is provided by the utility model for a kind of way of realization in the device for making technical field of formic acid; according to other distortion of scheme provided by the utility model; increase or reduce composition or step wherein; or the technical field approaching with the utility model by the utility model for other, all belongs to protection domain of the present utility model.
Claims (5)
1. the device for making for formic acid, it is characterized in that: the device for making body that includes the formic acid of there is premixer (3), hydrolysis reactor (6), rectifying tower I (7) and rectifying tower II (12), wherein, for water and the mixed premixer (3) of methyl-formiate, the hydrolysis reactor (6) being communicated with premixer (3), the rectifying tower I (7) being communicated with hydrolysis reactor (6), the rectifying tower II (12) that is communicated with rectifying tower I (7), the top delivery port end of rectifying tower II (12) is set to be communicated with the input aperture end of premixer (3).
2. the device for making for formic acid according to claim 1, it is characterized in that: the device for making body of formic acid also includes preheater (5), reboiler I (9), condenser I (10), reboiler II (14) and condenser II (15), the input aperture end of premixer (3) is set to be communicated with water pot and methyl-formiate tank respectively, premixer (3) delivery port end is set to be communicated with the input aperture end of hydrolysis reactor (6) by preheater (5), hydrolysis reactor (6) delivery port end is set to be communicated with the input aperture end of rectifying tower I (7), reboiler I (9) is set to be communicated with the heating source of rectifying tower I (7), the top gas delivery port end of rectifying tower I (7) is set to be communicated with the input aperture end of condenser I (10), the delivery port end of condenser I (10) is set to a road and is communicated with the input aperture end of rectifying tower I (7), another road is communicated with the input aperture end of methyl-formiate synthetic tower, the bottom delivery port end of rectifying tower I (7) is set to be communicated with the input aperture end of rectifying tower II (12) by the pump housing, reboiler II (14) is set to be communicated with the heating source of rectifying tower II (12), the top gas delivery port end of rectifying tower II (12) is set to be communicated with the input aperture end of condenser II (15), the delivery port end of condenser II (15) is set to a road and is communicated with the input aperture end of rectifying tower II (12), another road is communicated with the input aperture end of premixer (3), the bottom delivery port end of rectifying tower II (12) is set to be communicated with the input aperture end of formic acid finished pot by the pump housing.
3. the device for making for formic acid according to claim 2; It is characterized in that: rectifying tower I (7) is set to one-level rectifying tower, rectifying tower II (12) is set to two-stage rectification tower.
4. the device for making for formic acid according to claim 2; It is characterized in that: also include flash distillation plant (8), flash distillation plant (8) is arranged in rectifying tower I (7).
5. the device for making for formic acid according to claim 4; It is characterized in that: flash distillation plant (8) is set to include tank body (81), spray header (82) and wire packing layer (83), on the top end face of tank body (81), be provided with gaseous phase outlet and be provided with liquid-phase outlet on the bottom face of tank body (81), spray header (82) is arranged on the middle part of tank body (81), wire packing layer (83) is arranged on the gaseous phase outlet position of tank body (81), and spray header (82) is set to be communicated with hydrolysis reactor (6) delivery port end.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320530511.5U CN203683423U (en) | 2013-08-29 | 2013-08-29 | Preparation device used for formic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320530511.5U CN203683423U (en) | 2013-08-29 | 2013-08-29 | Preparation device used for formic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN203683423U true CN203683423U (en) | 2014-07-02 |
Family
ID=51005351
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201320530511.5U Expired - Lifetime CN203683423U (en) | 2013-08-29 | 2013-08-29 | Preparation device used for formic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN203683423U (en) |
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2013
- 2013-08-29 CN CN201320530511.5U patent/CN203683423U/en not_active Expired - Lifetime
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170906 Address after: 271612, Tai'an, Shandong province Feicheng Stone Town Middle and high Yu Cun Patentee after: SHANDONG ASIDE TECHNOLOGY CO.,LTD. Address before: 271600 Shandong city of Tai'an province Feicheng City West Street No. 121 Patentee before: FEICHENG ACID CHEMICALS CO.,LTD. |
|
| TR01 | Transfer of patent right | ||
| CX01 | Expiry of patent term |
Granted publication date: 20140702 |
|
| CX01 | Expiry of patent term |