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

Method for preparing cobalt-manganese-bromine composite aqueous solution by utilizing recycled cobalt manganese salt

An aqueous solution, cobalt-manganese technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve problems such as increased iron ion content, aggravated equipment corrosion, hidden dangers of production equipment, etc., to achieve simple operation Effect

Active Publication Date: 2018-03-02
浙江利星科技股份有限公司
View PDF7 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Because sodium carbonate and sodium hydroxide are all strong bases, therefore, in the process of implementing precipitation and washing cobalt-manganese precipitates, the pH rise and contact with air can easily lead to the change of cobalt and manganese ions, so that carbonate or hydrogen Part of the 2-valent cobalt-manganese ions in the oxide is converted into 3-valent cobalt ions and 4-valent manganese ions and exists in the state of ultrafine compounds, resulting in the process of preparing cobalt-manganese acetate by reacting with acetic acid, and some high-valent cobalt-manganese compounds cannot be dissolved. The existence of its ultra-fine state can easily pass through the filter material and enter the product, which not only brings hidden dangers to the production equipment, but also leads to a decline in the quality of terephthalic acid products after entering the system
In addition, recovering trivalent cobalt ions and tetravalent manganese ions in the cobalt-manganese compound can quickly partially oxidize the bromide ions in the fresh catalyst to free bromine in the catalyst preparation system, and the concentration of free bromine can reach 30-200 mg / kg. Part of the free bromine not only reduces the catalytic effect and increases catalyst consumption, but also aggravates equipment corrosion, resulting in an increase in the content of iron ions in the circulating mother liquor, and causing serious corrosion and damage to the PTA system equipment, especially the titanium reactor

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a reactor with a capacity of 1000ml, add 165g of cobalt, manganese content and 8.19% and 8.33% of the freshly prepared cobalt-manganese precipitate and 80g of water, and gradually add 69g of glacial acetic acid in batches under stirring to prevent overflow. After the addition is completed, heat up and the reactor tail gas enters the tail gas treatment system after passing through the reflux condensing device. When the temperature rises to 75°C, 6g of hydrogen peroxide with a concentration of 5% is added at a rate of 0.0015molH 2 o 2 min -1 · L -1 After the addition, continue to stir and react for 30 minutes, then add 165g of 48% hydrobromic acid and 1.65g of hydrazine hydrate, adjust the temperature to 80±5°C, continue the reaction for 60 minutes, filter to obtain an aqueous solution of cobalt manganese bromide, add water to adjust the total weight 465g, of which The cobalt content is 2.90%, the manganese content is 2.95%, and the bromine content is 16.82%. The cob...

Embodiment 2

[0021]In a reactor with a volume of 1000ml, add 165g of cobalt, manganese content of 8.19% and 8.33% of cobalt-manganese precipitate and 80g of water, gradually add 59g of glacial acetic acid under stirring, after the addition is completed, heat up, the reactor The tail gas enters the tail gas treatment system after passing through the reflux condensing device. When the temperature rises to 60°C, 14g of 5% peracetic acid is added at a rate of about 0.0018mol CH 3 COOOH·min -1 ·L -1 After the addition, continue to stir and react for 30min, then add 245g of 48% hydrobromic acid, 0.4g of hydrazine hydrate, 0.5g of acetaldehyde, 0.5g of propionic acid, and 1.0g of phenol, adjust the temperature to 80±5°C, continue the reaction for 45min, and filter , to obtain cobalt manganese bromine aqueous solution, add water to adjust the total weight of 545g, wherein the cobalt content is 2.48%, the manganese content is 2.51%, and the bromine content is 21.1%. The cobalt manganese bromine aq...

Embodiment 3

[0023] In a reactor with a volume of 500ml, add 165g of cobalt, manganese content of 8.19% and 8.33% cobalt-manganese precipitate and 60g of water, gradually add 90g of glacial acetic acid under stirring, after the addition is completed, heat up, the reactor The tail gas enters the tail gas treatment system after passing through the reflux condensing device. When the temperature rises to 50°C, 50g of 10% hydrogen peroxide is added at a rate of 0.06molH 2 o 2 min -1 ·L -1 After the addition, continue to stir and react for 30 minutes, then add 150g of 48% hydrobromic acid, 0.1g of formic acid, and 0.1g of ascorbic acid, adjust the temperature to 80±5°C, continue to react for 30 minutes, filter to obtain an aqueous solution of cobalt manganese bromide, add water to adjust the total weight 500g, wherein the cobalt content is 2.72%, the manganese content is 2.74%, and the bromine content is 14.3%. The cobalt, manganese and bromine aqueous solution can be directly returned to the ...

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

The invention relates to a method for preparing a cobalt-manganese-bromine aqueous solution by utilizing a cobalt manganese carbonate or / and hydroxide precipitate recycled from PTA (terephthalic acid)oxidation residues. The method comprises the following steps: adding the cobalt manganese carbonate or / and hydroxide into a reactor, adding acetic acid, adding hydrogen peroxide or peroxyacetic acid,performing a reaction to prepare a cobalt or / and manganese acetate aqueous solution, performing a reaction on the obtained aqueous solution, hydrobromic acid and 1-4 materials selected from formaldehyde, acetaldehyde, formic acid, phenol, hydrazine hydrate, ascorbic acid, oxalic acid, propionic acid, glucose, and a fructose to prepare the cobalt-manganese-bromine composite aqueous solution without containing free bromine, and the aqueous solution can be directly used for adjustment and preparation of a catalyst for preparing the terephthalic acid by oxidizing paraxylene.

Description

technical field [0001] The invention relates to the method field of preparing a cobalt-manganese-bromine composite aqueous solution by utilizing recovered cobalt-manganese. In more detail, the aqueous solution of alkali metal carbonate or / and hydroxide is added to the feed liquid containing cobalt-manganese discharged from the PTA device to obtain the precipitate of cobalt-manganese, and these precipitates are washed in acetic acid React directly with hydrogen peroxide or peracetic acid in the presence, and then react with 1 to 4 of hydrobromic acid and formaldehyde, acetaldehyde, formic acid, phenol, hydrazine hydrate, ascorbic acid, oxalic acid, propionic acid, glucose, and fructose A method for preparing a cobalt-manganese-bromine composite aqueous solution and recycling it. Background technique [0002] In the PTA production process, in order to control the quality of PTA products and prevent the accumulation of impurities, it is necessary to extract part of the oxidati...

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): B01J27/128
CPCB01J27/128
Inventor 曹善文李朝晖曹晓晴
Owner 浙江利星科技股份有限公司