Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation process and apparatus of high concentration anhydrous HBr/CH3 COOH agent

A high-concentration, reagent-based technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve increased processing difficulty, high cost, product quality and output limitations and other problems, to achieve the effect of preventing the reverse diffusion of water vapor, slowing down the reaction speed and strong dissolving ability

Inactive Publication Date: 2005-06-08
王心良
View PDF0 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the industrial synthesis method of hydrogen bromide gas is mostly red phosphorus hydrolysis, or hydrogen bromide gas is obtained while synthesizing certain organic substances such as dibromoaldehyde and brominated diphenyl ether. The cost of the former is too high, and the product quality and output of the latter Restricted
Due to the constraints of the preparation method, chemical reagent suppliers at home and abroad can only provide low-concentration HBr / CH 3 COOH reagents, including Sigma-Aldrich Catalog, can only provide acetic acid solutions with a maximum concentration of 33wt.% HBr, and they all have a certain water content. At present, there is no higher concentration or saturated solution available. Due to the low concentration, it directly affects Reagent selectivity, reaction speed, solubility and other properties, especially water content, a small amount of water can easily break peptide chains, nucleic acid chains or glycosidic bonds, increasing the difficulty of subsequent processing

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation process and apparatus of high concentration anhydrous HBr/CH3 COOH agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Such as figure 1 As shown, the device of the present invention comprises a gas generating device composed of a temperature controller 1 with a water bath device, a reaction tank 2, a constant pressure dropping funnel 3, an agitator 4, and a reflux condenser tube 5, and two connecting pipes are connected. Purification tanks 6 and 7, the two ends of the connecting pipe are close to the bottom of the tank, the purification tank 7 is connected with the gas absorption tank 9 through the communication pipe and the buffer bottle 8, a water bath 10 is arranged outside the absorption tank, and the gas absorption tank is connected to the double-stage drying tank through the connecting pipe. The towers 11 and 12 are connected, and the double-stage drying tower is connected with the tail gas absorption tower 13 . The two ends of each connecting pipe are preferably close to the bottom of the tank. The specific preparation method is as follows:

[0015] 1. Preparation of anhydrous ...

Embodiment 2

[0019] Embodiment 2: device is the same as embodiment 1, and concrete preparation method is as follows:

[0020] 1. Preparation of anhydrous acetic acid: freeze glacial acetic acid at 10°C, then pour or filter to remove unfrozen liquid, then melt in a warm water bath, transfer to a reflux distillation device and add 1.0% of the total weight of glacial acetic acid P 2 o 5 , and the reflux distillation unit was filled with molten solid KOH and anhydrous CaCl respectively 2 The two-stage drying tower is connected, and the reflux is distilled after 3 hours to obtain anhydrous acetic acid.

[0021] 2. Add 30 parts by weight of red phosphorus, CCl 4 35 parts by weight, 90 parts by weight of hydrobromic acid of 45%, respectively add 85% H to two scrubbing tanks 3 PO 4 35 parts by weight, P 2 o 5 4 parts by weight, 4 parts by weight of red phosphorus, add 110 parts by weight of anhydrous acetic acid to the absorption tank, successively connect the reaction tank (one end of the r...

Embodiment 3

[0024] Embodiment 3: device is the same as embodiment 1, and concrete preparation method is as follows:

[0025] 1. Preparation of anhydrous acetic acid: freeze glacial acetic acid at 6°C, then pour or filter to remove the unfrozen liquid, then melt it in a warm water bath, transfer to a reflux distillation device and add 0.9% of the total weight of glacial acetic acid P 2 o 5 , and the reflux distillation unit was filled with molten solid KOH and anhydrous CaCl respectively 2 The two-stage drying tower is connected, and the reflux is distilled after 2.5 hours to obtain anhydrous acetic acid.

[0026]2. Add 30 parts by weight of red phosphorus, CCl 4 30 parts by weight, 80 parts by weight of hydrobromic acid of 45%, respectively add 85%H to two scrubbing tanks 3 PO 4 30 parts by weight, P 2 o 5 5 parts by weight, 3 parts by weight of red phosphorus, add 100 parts by weight of anhydrous acetic acid to the absorption tank, successively connect the reaction tank (one end of...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

A process and apparatus for preparing the high-concentration anhydrous HBr / CH3COOh reagent is disclosed. Its process includes such steps as preparing anhydrous acetic acid, proportionally adding the red phosphorus, CCl4 and hydrobromic into reactor, the H3PO4, P2O5 and red phosphorus into two gas washing tanks, and the anhydrous acetic acid into absorptive tank, communicating all tanks in the system, adding the mixture of liquefied bromo and concentrated hydrobromic acid to dropping hopper, stirring while heating to slight boiling, and slow dropping said mixture while controlling temp to 30-80 deg.C by water bath until the bubbles are generated continuously.

Description

technical field [0001] The present invention relates to a kind of production method of chemical reagent, especially a kind of high concentration anhydrous HBr / CH 3 Preparation method and device of COOH reagent. Background technique [0002] Hydrogen bromide / acetic acid reagent is widely used in the fields of peptide, protein, nucleic acid synthesis, drug synthesis and organic chemical industry because of its good performance. It is an excellent reagent for some esterification reactions. At present, the industrial synthesis method of hydrogen bromide gas is mostly red phosphorus hydrolysis, or hydrogen bromide gas is obtained while synthesizing certain organic substances such as dibromoaldehyde and brominated diphenyl ether. The cost of the former is too high, and the product quality and output of the latter Restricted. Due to the constraints of the preparation method, chemical reagent suppliers at home and abroad can only provide low-concentration HBr / CH 3 COOH reagents,...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02
Inventor 王心良
Owner 王心良