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Method for simple detecting the stabilization of solid phosphoric acid catalyst

A phosphoric acid catalyst, catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical analysis by titration method, etc., can solve the problems of long reaction period, high labor intensity, large investment in equipment and manpower, etc.

Inactive Publication Date: 2005-02-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the shortcomings of the previous methods for measuring the stability of solid phosphoric acid catalysts, such as large equipment and manpower investment, long reaction cycle, cumbersome operation, and high labor intensity, and provide a simple method for measuring the stability of solid phosphoric acid catalysts. This method does not require reactors, instruments and other equipment and a large amount of manpower input, and has the characteristics of short measurement period, low labor intensity, reliable method and easy operation

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  • Method for simple detecting the stabilization of solid phosphoric acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The solid phosphoric acid catalyst A is pulverized so that the particle size of the catalyst is 50-80 mesh, and the composition of the catalyst A is calculated by molar ratio:

[0028] Si 1 B 0.8 (P 2 o 5 ) 1.5 ·(H 2 O) 0.87

[0029] 1. Catalyst A soaking for the first time:

[0030] Weigh 4 grams of the above-mentioned catalyst A in a 250 ml iodine measuring bottle, add 100 ml of detached water, place it in a constant temperature tank at 30°C, and soak for 2 hours to obtain the mixed soaking solution for the first soaking of the catalyst; The whole soaking solution is divided into 2 parts in equal volume, respectively moved into two 250 milliliter volumetric flasks, add 10 drops of 0.1% (weight) thyme phenolphthalein aqueous solution in each part as indicator, and use 0.5000 mol / liter of standard sodium hydroxide Solution titration, titration until the soaking solution is light green is the end point, record the volume of the consumed sodium ...

Embodiment 2

[0042] Stability Evaluation of Catalyst A.

[0043] Catalyst A is loaded into a stainless steel tubular reactor with an inner diameter of 25 mm, with a catalyst loading capacity of 100 ml and fillers up and down. Reaction raw material is made up of 85% (wt) butene-2 ​​and 15% (wt) butane, makes reaction raw material enter reactor and catalyzer contact by metering pump, at reaction temperature 180 ℃, reaction pressure 5.0MPa, liquid volume space velocity 2.0 hours -1 Carry out butene dimerization reaction under the conditions, continuous reaction for 576 hours, the material flowing out of the reactor after the reaction is analyzed by gas chromatography, the reaction time is 2, 24, 72, 144, 216, 288, 360, 432, 504, 576 hours Sampling and analysis (for ease of comparison, the sampling and analysis time is the same as the cumulative immersion time of catalyst A in Example 1), and the conversion of butene was calculated. The evaluation reaction results of Catalyst A are shown in ...

Embodiment 3

[0049] Take the solid phosphoric acid catalyst B and pulverize it so that its particle size is 50-80 mesh. The composition of the solid phosphoric acid catalyst B is calculated in molar ratio:

[0050] Si 1 Fe 0.30 B 0.86 (P 2 o 5 ) 1.50 ·(H 2 O) 0.75

[0051] Soak the catalyst B according to the method of Example 1, filter the soaking solution, titrate, calculate the total phosphoric acid content in the gained soaking solution after soaking the catalyst B for 2, 24, 72, 144, 216, 288, 360, 432, 504, 576 hours .

[0052] The stability evaluation method of catalyst B is the same as in Example 2.

[0053] See Table 3 for the soaking and evaluation reaction results of Catalyst B.

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Abstract

The method of simply testing the stability of solid phosphoric acid catalyst includes several times of soaking the catalyst in water, filtering and alkali titrating the mixed acid soaking solution obtained through each soaking, calculating the phosphoric acid content of the each soaking solution, and accumulating the leached phosphoric acid content for evaluating the stability of the catalyst. The higher the total leached phosphoric acid content, the higher the stability of the catalyst. When the catalyst is soaked for 15 days totally and the total leached phosphoric acid content is higher than 40 % in the mass of P2O5, the catalyst is considered to have better stability. The said method has the features of short test period, low labor strength, high reliability and simple operation.

Description

technical field [0001] The invention relates to a method for simply measuring the stability of a solid phosphoric acid catalyst, in particular to a method for simply measuring the stability of a solid phosphoric acid catalyst with a chemical analysis method. Background technique [0002] Solid phosphoric acid catalyst (SPAC) is a catalyst widely used in the petrochemical industry. It has decades of industrial application history in the fields of oligomerization, superposition, alkylation, and hydration of low-carbon olefins. Traditional solid phosphoric acid catalysts mainly include P and Si components are prepared from polymerized phosphoric acid and diatomaceous earth. The subsequent improved catalyst is based on the traditional solid phosphoric acid catalyst, and is made by adding a small amount of boron, iron, chromium, magnesium and other elements. Due to its low price, The advantages of loose requirements on raw materials and low total pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/16B01J27/182B01J27/185G01N31/16
Inventor 金萍袁梅卿姚亚平徐菁陈永福
Owner CHINA PETROLEUM & CHEM CORP