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Method for removing catalyst from unsaturated copolymer hydrogenated solution

A technology of copolymer and catalyst, which is applied in the field of catalyst removal in unsaturated copolymer hydrogenation solution, can solve the problems of long time, low one-time removal rate, insufficient precious metal catalyst removal rate, etc.

Inactive Publication Date: 2004-03-24
NANTEX IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the one-time removal rate is low, and repeated kneading and extraction are required, and the operation is cumbersome and takes a long time; (2) precipitation method
Its disadvantage is that the removal rate of the ruthenium noble metal catalyst is not high enough, and the removal of organic ligands is not mentioned

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] According to the above general procedure for catalyst removal, take 20ml of hydrogenated nitrile copolymer (HNBR) rubber solution No. 2 in Table 1 and place it in the reactor, add 40ml of triethanolamine aqueous solution with a concentration of 21.5% at about 100-120 rpm. It was stirred for minutes and the temperature was raised to 80°C, and then 10 ml of a 30% hydrogen peroxide aqueous solution was added, and the reaction was kept constant for 2 hours under stirring. After the reaction is completed, the reaction mixture is naturally separated by cooling, and the extractant aqueous solution is separated from the HNBR rubber solution. Take the extract and analyze the concentration of metal rhodium in the catalyst. It is determined that the removal rate of the rhodium catalyst in the HNBR rubber solution is 98.0%.

Embodiment 2-6

[0051] Repeat Example 1. Add the HNBR rubber solution of No. 2 in Table 1 to the reactor, select different peroxides and extractants, and their amounts. After the reaction, the extractant aqueous solution and the rubber solution are separated into phases, and the extractant aqueous solution is analyzed. The metal rhodium concentration of the catalyst in the HNBR, the removal rate of the rhodium catalyst in the HNBR rubber solution was measured, as shown in Table 2.

[0052] Example

2

3

4

5

6

Rubber solution volume, ml

40

40

20

20

20

Extractant concentration,%

13.2% formic acid

36.0% acetic acid

36.0% acetic acid

33.0% acetic acid

10.6% TriB

Alcoholamine

The amount of extractant, ml

40

40

20

20

40

Peroxide concentration%

30%H 2 O 2

30%H 2 O 2

30% peracetic acid

Ethanol solution

30% persulfuric acid...

Embodiment 7-13

[0056] Repeat Example 1. Add the HNBR rubber solution in Table 1 to the reactor. The difference is that the peroxide and its amount are different, or the concentration of the extractant is different. After the reaction, the aqueous solution of the extractant and the rubber solution are separated and the extraction is analyzed. The concentration of rhodium and ruthenium metal of the catalyst in the solution, and the removal rate of rhodium or rhodium and ruthenium of the catalyst in the HNBR rubber solution were measured. See Tables 3 and 4.

[0057] Example

7

8

HNBR rubber solution

Number 5 in Table 1

Number 3 in Table 1

HNBR rubber solution volume, ml

20

20

Extractant concentration,%

33% acetic acid

33% acetic acid

The amount of extractant, ml

20

40

Peroxide concentration,%

30% ammonium persulfate

30% ammonium persulfate

Peroxide amount, ml

5.0

...

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PUM

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Abstract

The present ivnention provides a method for removing rhodium and / or ruthenium catalyst from unsaturated copolymer homogeneous hydrogenated solution, and is characterized by that it makes the peroxide, aqueous solution of extraction agent and hydrogenated solution of the unsaturated copolymer produce reaction together to extract the rhodium and / or ruthenium catalyst into the aqueous solution, and separate them from copolymer solution. In the butadiene-acrylonitrile copolymer hydrogenated solution in which the rhodium organic coordination compound is used as catalyst the one-step removing rate of rhodium can be up to above 98.8%, and in the butadiene-acrylonitrile copolymer hydrogenated solution using rhodium and ruthenium bimetal organic coordination compound as catalyst the one-step removing rates of rhodium and ruthenium can be respectively up to 99.9% and 98.3%.

Description

Technical field [0001] The invention provides a method for removing rhodium or / and ruthenium noble metal catalyst and its organophosphine ligand from a viscous unsaturated copolymer hydrogenation solution into an aqueous extractant solution by using a peroxide and a water-soluble extractant It is especially suitable for the removal of rhodium or / and ruthenium noble metal catalysts and their organophosphine ligands in the homogeneous hydrogenation solution of butadiene-acrylonitrile copolymers. Background technique [0002] Unsaturated copolymers such as butadiene-acrylonitrile copolymers contain carbon-carbon double bonds (C=C) in their molecular chains, and their heat resistance, aging resistance, and corrosion resistance are affected, which limits their application fields. After selective hydrogenation of carbon-carbon double bonds, especially carbon-carbon double bonds containing nitrile groups, the aging properties such as heat resistance, acid fuel resi...

Claims

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Application Information

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IPC IPC(8): C08C19/02
Inventor 许贵显毛倩瑾姚明岳冬梅徐瑞清
Owner NANTEX IND
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