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Method for preparing formic acid by acidifying sodium formate with acidification adjuvant

A technology of sodium formate and additives, which is applied in the field of formic acid preparation, can solve the problems of formic acid quality decline, lower formic acid concentration, and many by-products, and achieve the effects of reducing production costs, optimizing the operating environment, and facilitating operation

Active Publication Date: 2008-03-12
YIBIN TIANYUAN GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since acidification is an exothermic reaction, and formic acid is easy to decompose under local overheating, producing carbon monoxide and water; if the decomposition temperature is greater than 100°C, formic acid will be oxidized to produce carbon dioxide and water, and the resulting water will cause the concentration of formic acid to be low. High-concentration formic acid of more than 95% cannot be obtained; further, sodium carbonate will be produced, which will not only greatly reduce the concentration of formic acid, but also bring about many by-products, a decline in the quality of formic acid and serious problems of three wastes
[0003] Chinese patent 200610200857.3 discloses a method for preparing 95% high-concentration formic acid. It uses a reducing multi-component polymeric phosphoric acid mixture as an acidulant to acidify sodium formate to produce 95% high-concentration formic acid. The principle is to use a polymeric phosphoric acid mixture The high adsorption performance absorbs the moisture in the reaction system, thereby increasing the concentration of formic acid. However, the disadvantage of this process is that the amount of polymerized phosphoric acid mixture used will increase, and it may also absorb a certain amount of formic acid. Although it is said to be able to obtain 95% high Concentration of formic acid, but in the actual production process, it is far from reaching this concentration. In addition, its subsequent treatment process is more complicated than traditional technology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: in reactor, add anhydrous sodium formate, add the pentane of 40-60 ℃ of boiling range 40-60 ℃ of sodium formate charging amount 6%, meter the sulfuric acid that adds 98%, reaction heat is taken out reactor by pentane gasification, The temperature is lowered by 10-20°C cooling water, and then returned to the reactor after condensation. When the metered 98% sulfuric acid drop rate is controlled for 1-2 hours, continue to react for 20-30 minutes after adding, until there is no back distillation, the solvent is distilled off at 80°C, and the late stage is steamed in a low vacuum until the formic acid is distilled, and the recovered ammonium Alkane and a small amount of formic acid are used for the next batch of sodium formate acidification reaction, and the solvent recovery rate is greater than 96%. The formic acid is distilled out of the reaction material after the solvent is removed under an absolute pressure of 0.03-0.04 MPa, the formic acid content is grea...

Embodiment 2

[0020] Embodiment 2: In the reactor, add anhydrous sodium formate, add the cyclopentane of sodium formate charging amount 6%, meter and add 100% phosphoric acid (available 85% phosphoric acid and the superphosphoric acid mixing preparation of 105%) react at 60 ± 5 ℃ , the heat of reaction is taken out of the reactor by cyclopentane vaporization, cooled by 10-20°C cooling water, and returned to the reactor after condensation. The 100% phosphoric acid addition rate is controlled for 1-2 hours, and the reaction is continued for 20-30 minutes after the addition is completed. Upright without back distillation, solvent is distilled at 80°C, low vacuum is used to distill formic acid in the later stage, cyclopentane and a small amount of formic acid are recovered, and used for the next batch of sodium formate acidification reaction, the solvent recovery rate is greater than 96%, and the solvent is completely removed. The formic acid is distilled from the material under an absolute pres...

Embodiment 3

[0021] Embodiment 3: in reactor, add anhydrous sodium formate, add sodium formate charging amount 8% isopropyl ether, meter and add 100% phosphoric acid, react below 80 ℃, reaction heat is taken out reactor by isopropyl ether vaporization, by 20 ℃ Cooling water to cool down, return to the reactor after condensation, 100% phosphoric acid drop rate is controlled for 1-2 hours, continue to react for 20-30 minutes after the addition, stand upright without back distillation, distill isopropyl ether below 80 ℃, and later in Distill a small amount of isopropyl ether under 50MPa absolute pressure until the formic acid is distilled, and recover the isopropyl ether for the next reaction. The solvent recovery rate is greater than 96%. After the solvent is removed, the reaction material is distilled under 0.03-0.04MPa absolute pressure. Formic acid, the formic acid content is greater than 96%, and the yield is greater than 98%.

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Abstract

The present invention discloses a method of using the acidification of the sodium formate with the acidified assistant reagent to prepare the formic acid. In the method, the inhibitor is added in the reaction process; the inhibitor is at least one of the alkane, cycloalkane, ether or a formic ester whose boiling point is below 80 DEG C. The present invention can effectively control the reaction temperature, inhabit the side reaction and obtain the formic acid whose collection rate is 98 percent; the formic acid of the high concentration can be prepared with the concentration of 98 percent. Besides, the operation is convenient, safe and economical; the present invention can effectively control the environmental pollution.

Description

technical field [0001] The invention relates to a method for preparing formic acid, in particular to a method for preparing formic acid by acidifying sodium formate with an acidifying auxiliary agent. Background technique [0002] It is known that to prepare formic acid from sodium formate, sulfuric acid, phosphoric acid, superphosphoric acid or polymeric phosphoric acid, phosphorus pentoxide and other acidifying aids can be added to acidify to prepare formic acid. The methods for preparing formic acid, these methods have been tested by production practices are practical and effective. However, since acidification is an exothermic reaction, and formic acid is easy to decompose under local overheating, producing carbon monoxide and water; if the decomposition temperature is greater than 100°C, formic acid will be oxidized to produce carbon dioxide and water, and the resulting water will cause the concentration of formic acid to be low. High-concentration formic acid above 95...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/02C07C51/02
CPCC07C51/02
Inventor 罗云曹正祥邓敏
Owner YIBIN TIANYUAN GRP CO LTD