Novel purification method for formic acid

A new method, formic acid technology, is applied in the field of formic acid purification, which can solve the problems of environmental pollution, high cost, and large consumption of entrainer, and achieve the effects of reduced process cost, easy distillation temperature, and low energy consumption

Active Publication Date: 2012-01-11
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The principle of this method is that phthalic anhydride can selectively react with water to form phthalic acid, thereby removing the water in formic acid. However, the disadvantage of this method is that a large amount of phthalic acid formed by the reaction is difficult to recycle. Economic and environmental pressures
Add new entrainer in aqueous formic acid as British patent report in 1948, the obvious shortcoming of this type of method is: entrainer propyl formate, isobutyl formate etc. generally need to be prepared from anhydrous formic acid, simultaneously The consumption of entrainer is also relatively large, and the production cost is relatively high
Another example is the Chinese patent report in 1992, using SOCL 2 The principle of purifying dilute formic acid is that water in dilute formic acid and sulfite chloride selectively form hydrogen chloride and sulfur dioxide. Although this method can obtain high-concentration formic acid, it will cause certain pollution to the environment, and it will bring more problems in industrial implementation. high cost
Another example is the boric anhydride purification method reported in Chinese literature in 2006. Its principle boric anhydride (boron trioxide) reacts with water in dilute formic acid to form boric acid. After distillation, high-concentration formic acid can be obtained. Reuse, but boric acid is dried and dehydrated into boric anhydride, which can only be carried out at a temperature above 300°C, which is difficult to implement industrially, and boric anhydride is expensive, and the production cost is too high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In the 2000 milliliter three-necked round-bottomed flask that has constant temperature oil bath, thermometer, electric stirring, add 1554 grams (14.0 mole) calcium chloride anhydrous, then add the formic acid solution 800 grams of content 50% (wherein formic acid contains the substance of water The amount is 22.2 moles), and at a temperature of 80 to 95° C., heated and stirred for 5 hours to dissolve calcium chloride. After the calcium chloride is dissolved, distill under normal pressure and collect fractions at 100-106°C. 409.6 g of formic acid with a content of 91.6% was obtained, and the recovery rate of formic acid was 93.8%. The remaining calcium chloride solution is subjected to vacuum distillation and dehydration at a temperature of 150-180° C. and a vacuum degree of 0.09-0.095 MPa to evaporate the calcium chloride to dryness and apply it to the next batch.

Embodiment 2

[0023] Add 830 grams (7.5 moles) of anhydrous calcium chloride in a 1000 milliliter three-neck round bottom flask with constant temperature oil bath, thermometer and electric stirring, then add 400 grams of formic acid solution with a content of 44% (wherein the formic acid contains water The amount is 12.4 moles), at a temperature of 80-95°C, heated and stirred for 4 hours to dissolve calcium chloride, after the calcium chloride was dissolved, distilled at atmospheric pressure, collected 100-106°C cuts, and obtained 181.6 grams with a content of 91.1% formic acid, formic acid recovery rate 94.0%. The remaining calcium chloride solution is subjected to vacuum distillation and dehydration at a temperature of 150-180° C. and a vacuum degree of 0.09-0.095 MPa to evaporate the calcium chloride to dryness and apply it to the next batch.

Embodiment 3

[0025] Add 365 grams (3.3 moles) of anhydrous calcium chloride in a 500 milliliter three-necked round-bottomed flask with constant temperature oil bath, thermometer and electric stirring, then add 160 grams of formic acid solution with a content of 40% (the substance containing water in the formic acid The amount is 5.3 moles), at a temperature of 80-95°C, heat and stir for 4 hours to dissolve calcium chloride, after the calcium chloride is dissolved, distill at atmospheric pressure, collect the fraction at 100-106°C, and obtain 65.9 grams of 90.8% formic acid, formic acid recovery rate is 93.5%. The remaining calcium chloride solution is subjected to vacuum distillation and dehydration at a temperature of 150-180° C. and a vacuum degree of 0.09-0.095 MPa to evaporate the calcium chloride to dryness and apply it to the next batch.

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Abstract

The invention discloses a new method for formic acid purifying, which comprises the following steps: the aqueous solution of dilute formic acid with the mass concentration of more than 30 percent and anhydrous calcium chloride are mixed, heated to 80 distillation; and the mass ratio of the water in the aqueous solution of calcium chloride anhydrous and the aqueous solution of dilute formic acid is 1: 1.5 to 95 DEG C so as to lead the anhydrous calcium chloride to be dissolved, and then formic acid with high concentration is obtained through atmosphericto 1.8. The purifying method of formic acid is a process which has the advantages of simple and convenient operation, fastness, low cost and cleanness, thus being suitable for industrial production.

Description

(1) Technical field [0001] The invention relates to a new technology for purifying formic acid. (2) Background technology [0002] Formic acid, commonly known as formic acid, is a colorless liquid with a boiling point of 100.7°C and a melting point of 8.4°C. Formic acid is used as reducing agent, condensation agent, formylation reagent and solvent in synthesis. [0003] In the past, methods for purifying formic acid have been reported in the literature. For example, the French patent report in 1929 prepared anhydrous formic acid by reflux reaction of phthalic anhydride and aqueous formic acid. The principle of this method is that phthalic anhydride can selectively react with water to form phthalic acid, thereby removing the water in formic acid. However, the disadvantage of this method is that a large amount of phthalic acid formed by the reaction is difficult to recycle. Economic and environmental protection pressures. Add new entrainer in aqueous formic acid as British...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/02C07C51/42
Inventor 丁成荣许莉张翼贺孝啸谢思泽来虎钦
Owner ZHEJIANG UNIV OF TECH
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