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Method for testing content of alkyl chloride aluminum for ethylene-propylene polymerization

A technology of alkylaluminum chloride and ethylene propylene, which is applied in the field of ethylene-propylene rubber, can solve problems such as inconvenient operation, inaccurate testing, and rough hydrolysis treatment and absorption methods, and achieve the effect of simple and easy method and accurate test results

Inactive Publication Date: 2018-06-29
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The hydrolysis treatment step needs to be carried out in a nitrogen box, which is inconvenient to operate
Moreover, the absorption method of hydrolysis treatment is rough, and the absorption of hydrogen chloride gas is not complete, which can easily lead to inaccurate testing, and the test results can only be used as a reference

Method used

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  • Method for testing content of alkyl chloride aluminum for ethylene-propylene polymerization
  • Method for testing content of alkyl chloride aluminum for ethylene-propylene polymerization
  • Method for testing content of alkyl chloride aluminum for ethylene-propylene polymerization

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment approach

[0057] (1) Hydrolysis treatment:

[0058] Replace the dried vessel 1 with nitrogen gas, connect the glass tubes on both sides to the latex tubes, clamp them with water-stop clamps, add 30mL of anhydrous ether, and weigh to an accuracy of 0.0002g. Use a 5-10mL glass syringe to add 2-10mL of the alkylaluminum chloride sample to be tested from one side of the latex tube, weigh to an accuracy of 0.0002g, and the difference between the two weights is the sample weight.

[0059] Connect the latex tube on one side of the container 1 to the water washing device, that is, two water washing bottles connected in series. Slowly add 5-15mL of 5-15% sulfuric acid from the unconnected side. Do not generate a lot of air bubbles during this process. After the hydrolysis reaction is complete, transfer all the liquid to a 250mL volumetric flask, and rinse the absorption bottle and vessel 1 with water. Pour into a volumetric flask. After fully shaking, stand still for 5 minutes, and finally use...

Embodiment 1

[0097] Hydrolysis treatment:

[0098] Replace the dried 50mL container 1 with nitrogen, connect the glass tubes on both sides to the latex tubes, clamp them with water-stop clips, add 30mL of anhydrous ether, and weigh them, and the weight is 91.3308g. Use a 10mL glass syringe to add 4mL of ethylaluminum sesquichloride to be tested from one side of the latex tube, weigh it, the weight is 94.3808g, and the difference between the two weights is the sample weight is 3.0500g.

[0099] Connect the latex tube on one side of the container 1 to the water washing device, that is, two water washing bottles connected in series. Slowly add 10mL of 8% sulfuric acid from the unconnected side, bubbles appear slowly, the hydrolysis reaction is complete, and no bubbles appear, transfer all the liquid to a 250mL volumetric flask, rinse the absorption bottle and vessel 1 with water, and pour all the rinse water into the volumetric flask bottle. After fully shaking, stand still for 5 minutes, a...

Embodiment 2

[0107] Hydrolysis treatment:

[0108] Replace the dried 50mL vessel 1 with nitrogen gas, connect the glass tubes on both sides to the latex tubes, clamp them with water-stop clamps, add 30mL of anhydrous ether, weigh, and the weight is 88.2289g. Use a 5mL glass syringe to add 2mL of ethylaluminum sesquichloride to be tested from one side of the latex tube, weigh it, the weight is 89.6309g, the difference between the two weights is the sample weight is 1.402g.

[0109] Connect the latex tube on one side of the container 1 to the water washing device, that is, two water washing bottles connected in series. Slowly add 15mL of 10% sulfuric acid from the unconnected side, bubbles appear slowly, the hydrolysis reaction is complete, and no bubbles appear, transfer all the liquid to a 250 volumetric flask, rinse the absorption bottle and vessel 1 with water, and pour all the rinse water into the volumetric flask bottle. After fully shaking, stand still for 5 minutes, and finally use...

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Abstract

The invention discloses a method for testing the content of alkyl chloride aluminum for ethylene-propylene polymerization. The method comprises the following steps: performing dehydration treatment onalkyl chloride aluminum in a vessel, performing titration to test the content of aluminum by using a complexing titration method, and further performing titration to test the content of chloride by using a Volhard method. By adopting the method, a conventional alkyl chloride aluminum content testing method is changed, the method does not need to be carried out in a nitrogen tank, and only reactions and hydration treatment are carried out in a ventilation cabinet. The method is simple, convenient and feasible. The hydration treatment steps are carried out in relatively special vessels, an alkyl chloride aluminum sample is added in a completely sealed environment in the testing process, the sample and a hydrogen chloride gas generated from reactions are not lost, and precise testing resultscan be achieved.

Description

technical field [0001] The invention belongs to the technical field of ethylene-propylene rubber, in particular to a method for determining the content of alkylaluminum chloride for ethylene-propylene polymerization. Background technique [0002] The most traditional catalytic system used in solution polymerization ethylene propylene rubber technology is Ziegler-Natta (Ziegler-Natta) system, mainly composed of transition metal vanadium, titanium compounds and alkyl aluminum compounds (also known as V-Al system) , mostly using vanadium oxychloride as the main catalyst, alkylaluminum sesquihalide as the co-catalyst, and an activator or accelerator to improve the catalyst activity as the catalytic system. where VOCl 3 -1 / 2Al 2 (C 2 h 5 ) 3 Cl 3 The combined catalyst system is the most common, and it is also the basic catalytic system for the production of ethylene-propylene rubber by solution polymerization in industry. [0003] The alkylaluminum chloride used as a cocat...

Claims

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Application Information

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IPC IPC(8): G01N31/16
CPCG01N31/16
Inventor 张柳隋军范玉丽单振国高虹周树侠邵信壮王刚温冬梅
Owner PETROCHINA CO LTD
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