Technique of manufacturing trifluoro acetic anhydride

A technology of trifluoroacetic anhydride and trifluoroacetic acid, which is applied in the field of preparing trifluoroacetic anhydride and achieves the effects of reducing product loss, convenient operation and good heating effect

Inactive Publication Date: 2008-01-23
申厚宝
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the deficiencies of the existing production process, and provide a production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 200 kilograms of phosphorus pentoxide with a content of 98.20% (mass percentage, the same below), put 189.7 kilograms of it into a clean, dry 500-liter reactor, and introduce 250 kilograms of measured trifluoroacetic acid with a content of 98.5% In the high drop tank. Check that the sealing of each interface is good, and the emptying pipeline of the top of the distillation tower and the receiving tank is unblocked. Turn on the deep well water pump to feed condensed water into the condenser to circulate, start to add phosphorus pentoxide dropwise at a rate of 0.15 liters / minute, adjust the dropping rate to 0.4 liters / minute after 10 minutes, and adjust it to 0.8 liters / minute after 10 minutes. Adjust to 1.2 liters / minute after 10 minutes, adjust to 1.8 liters / minute after 10 minutes, adjust to 2.8 liters / minute after 10 minutes, adjust to 3.8 liters / minute after 10 minutes, until the dropwise addition is completed, close the dripping pipeline valve. At this time, ...

Embodiment 2

[0028] Weigh 210 kilograms of phosphorus pentoxide with a content of 98.15% (mass percentage, the same below), put 199.38 kilograms of it into a 500-liter reactor, and introduce 250 kilograms of trifluoroacetic acid with a measured content of 98.5% into the high-level dropwise Groove, the operation of following process (1) is the same as embodiment 1, wherein in the reflux reaction, the rate of addition of phosphorus pentoxide begins to be 0.2 liters / minute, and is adjusted to 0.6 liters / minute, 1.0 liters / minute every 10 minutes afterwards , 1.6 liters / minute, 2.0 liters / minute, 3.0 liters / minute, 4.0 liters / minute, until the dropwise addition is completed; in the process of recovering the by-product phosphoric acid, add 150 kilograms of metered recovery steam condensate dropwise, and the dropping rate starts to be 0.4 L / min, adjust to 0.8 L / min after 20 minutes, adjust to 2.0 L / min after 20 minutes, until the addition is complete.

[0029] In this process (1), 143 liters of ...

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PUM

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Abstract

A trifluoroacetic anhydride processing technique is provided, which utilizes the trifluoroacetic acid and the phosphorus pentoxide as raw materials. The material usage rate (weight) of the trifluoroacetic acid and the phosphorus pentoxide is 1 : 1.5 to 1 : 0.65 and the phosphorus pentoxide is added twice. The entire operation process is done in the fully sealed state, the high boiling substance (after cut) and the tail gas are treated and recycled after collecting the finished products; the condensing water and the cooling water are water from deep well and the byproduct phosphoric acid are all recycled. The invention prepares the trifluoroacetic anhydride applied in the highly efficient liquid chromatogram and the derivating agent of the gas chromatogram, the solvent, catalyst, the condensation dehydration agent and the retention agent of various synthetic reaction, which has complete, canonical and reasonable process and convenient operation, therefore is suitable for industrial production, can effectively improve the purity and the yield of the products, has no environment pollution and reduces the production cost.

Description

technical field [0001] The invention relates to a method for preparing trifluoroacetic anhydride by using trifluoroacetic acid and phosphorus pentoxide as raw materials. Background technique [0002] Trifluoroacetic anhydride (TFAA) is a strong dehydrating agent with a wide range of chemical reactivity. It is used as a solvent, catalyst, dehydration condensation agent and retention agent in the synthesis of various polymers and fine chemicals. It is widely used in dyes. , photosensitive materials, liquid crystal display materials, aerospace technology, pesticides, medicine, polymer materials, etc., to increase the speed of polymerization and the yield of products, and as a derivative chemical reagent for gas chromatography and high performance liquid chromatography in livestock meat, fruits and vegetables The detection of toxic metabolites and mycocins has very good development and application prospects. [0003] At present, there are many methods for synthesizing trifluoro...

Claims

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Application Information

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IPC IPC(8): C07C53/18C07C51/56
Inventor 申厚宝王泉民申少星尤小文
Owner 申厚宝
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