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Method for determining the content of normax catalyst and its ligand

A catalyst and ligand technology, applied in the field of 2-propyl heptanol production, can solve problems such as inaccurate results, and achieve the effects of accurate results and production cost savings

Active Publication Date: 2019-04-09
CHINA SHENHUA ENERGY CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Main purpose of the present invention is to provide a kind of method for measuring the content of NORMAX catalyst and its ligand, to solve the problem of adopting existing methods to carry out the content of NORMAX catalyst and its ligand in the 2-propylheptanol carbonylation reactor solution The problem of inaccurate results when testing

Method used

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  • Method for determining the content of normax catalyst and its ligand
  • Method for determining the content of normax catalyst and its ligand
  • Method for determining the content of normax catalyst and its ligand

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) Preparation of diluent

[0027] Nitrogen is passed into tetraethylene glycol dimethyl ether for degassing to obtain degassed tetraethylene glycol dimethyl ether;

[0028] In a nitrogen glove box, 1.00 g of diphenylcyclohexylphosphine was weighed and placed in a 100 mL glass bottle replaced with nitrogen, and degassed tetraethylene glycol dimethyl ether was added to the above glass bottle to make the diphenyl cyclohexyl phosphine Hexylphosphine was diluted to 100.00g, sealed, and shaken well to dissolve it to obtain the required dilution.

[0029] 2) Preparation of standard solution

[0030] In a nitrogen glove box, weigh 0.1197g of 3,3',5,5'-tetra-tert-butyl-2,2'-diphenol into a nitrogen-substituted 100mL glass bottle, and add to the glass bottle Add dilute solution to 3,3',5,5'-tetra-tert-butyl-2,2'-diphenol to be diluted to 100.0000g, seal and shake well to obtain standard solution, concentration C STD = 0.1197%.

[0031] 3) Calibration process

[0032] Accord...

Embodiment 2

[0039] 1) Preparation of diluent

[0040] Nitrogen is passed into tetraethylene glycol dimethyl ether for degassing to obtain degassed tetraethylene glycol dimethyl ether;

[0041] In a nitrogen glove box, 1.00 g of diphenylcyclohexylphosphine was weighed and placed in a 100 mL glass bottle replaced with nitrogen, and degassed tetraethylene glycol dimethyl ether was added to the above glass bottle to make the diphenyl cyclohexyl phosphine Hexylphosphine was diluted to 100.00g, sealed, and shaken well to dissolve it to obtain the required dilution.

[0042] 2) Preparation of standard solution

[0043] In a nitrogen glove box, weigh 0.1197g of 3,3',5,5'-tetra-tert-butyl-2,2'-diphenol (CAS: 6390-69-8) into a nitrogen-purged glass In the bottle, add diluent solution to dilute to 100.00g, seal and shake well to obtain standard solution, concentration C STD = 0.1197%.

[0044] 3) Calibration process

[0045] According to the chromatographic condition in claim 1, standard sample...

Embodiment 3

[0051] 1) Preparation of diluent

[0052] Nitrogen is passed into tetraethylene glycol dimethyl ether for degassing to obtain degassed tetraethylene glycol dimethyl ether;

[0053] In a nitrogen glove box, 1.00 g of diphenylcyclohexylphosphine was weighed and placed in a 100 mL glass bottle replaced with nitrogen, and degassed tetraethylene glycol dimethyl ether was added to the above glass bottle to make the diphenyl cyclohexyl phosphine Hexylphosphine was diluted to 100.00g, sealed, and shaken well to dissolve it to obtain the required dilution.

[0054] 2) Preparation of standard solution

[0055] In a nitrogen glove box, weigh 0.1065g of 3,3',5,5'-tetra-tert-butyl-2,2'-diphenol into a nitrogen-substituted 100mL glass bottle, and add to the glass bottle Add dilute solution to 3,3',5,5'-tetra-tert-butyl-2,2'-diphenol to be diluted to 100.00g, seal and shake well to obtain standard solution, concentration C STD = 0.1065 wt%.

[0056] 3) Calibration process

[0057] Accor...

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Abstract

The invention provides a method for measuring content of NORMAX catalyst and its ligand. The method includes preparing a sample solution, correcting, and detecting the sample. The content of NORMAX catalyst and its ligand is detected by using liquid chromatography, suitable liquid chromatographic conditions are acquired by the inventor through creative labor, and the measured results are more accurate under the above specific liquid chromatographic conditions. The content of the NORMAX catalyst and its ligand can be measured in time during production, the process can be adjusted in time according to detection results, and production cost can be saved.

Description

technical field [0001] The invention relates to the field of 2-propylheptanol production, in particular to a method for determining the content of a NORMAX catalyst and its ligand. Background technique [0002] The by-product of the MTO unit is relatively cheap mixed butene. After the raw material pretreatment MTBE / butene-1 unit, the total content of 1-butene and 2-butene is about 90wt%, which is an important factor for the production of 2-propyl Heptanol products provide an abundant and inexpensive raw material. A rhodium / NORMAX catalyst is required during the oxo reaction of 2-propylheptanol. The catalyst adopts bulky ligands, so that the reaction speed of olefins and the selectivity of normal products are greatly improved. The above reactions are carried out in three series-connected stirred liquid phase reactors, and the amount of NORMAX catalyst plays a crucial role in the carbonylation reaction, so timely and accurate analysis of the content of NORMAX catalyst become...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N1/14
CPCG01N1/14G01N30/02G01N2001/1463
Inventor 刘文星张维斌王春江赵安帮徐向文
Owner CHINA SHENHUA ENERGY CO LTD
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