SU1528542A1 - Method of cleaning hydrogen from oxygen admixtures - Google Patents

Abstract

The invention relates to the complex purification of hydrogen from mercury impurities and oxygen. To increase the degree of hydrogen purification from oxygen impurities and to ensure the simultaneous purification of mercury impurities in the first stage of the process, adsorption purification of hydrogen from mercury is performed, and in the second stage, catalytic purification of hydrogen from oxygen, using the adsorbent in the first stage and the stages of the purification process are the same reagent - a PD-containing K-PG catalyst, worked up during the hydrogenation of acetylene hydrocarbons in the C ₄ fraction. The process is carried out at atmospheric pressure, temperatures of 25-100 ° C and flow rates of the gas to be purified 1000-5000 h ^-1 . The method allows to bring the residual mercury content in hydrogen to 0%, and the residual oxygen content to 0.035%. 1 tab.

Description

The invention relates to the complex purification of hydrogen from mercury impurities and oxygen.

The purpose of the invention is to increase the degree of cleaning and to ensure the simultaneous removal of mercury impurities.

As an adsorbent for purifying hydrogen from mercury and a catalyst for purifying hydrogen from oxygen, use a Pd-containing K-PG catalyst (TU 38-10216-78), which has been used in the process of hydrogenation of acetylene hydrocarbons in fraction C. The catalyst has the following composition (wt.%) and properties:

Pd content, wt.% 1.2-1.4

(. content, wt;% 62.7 - 62.5 Content of resins,% 22.8

Moisture content,% 13.3

Bulk weight, g / cm 0,653

Specific surface, m / g77.4

Porosity,% 52,5

Pore radius, A1.1

Adhesional abrasion resistance (residue),% 7.5

The method is carried out as follows.

Example 1. The process is carried out in a two-stage reactor, in the first stage of which mercury is adsorbed and in the second stage catalytic oxygen reduction is carried out.

The volumetric feed rate of hydrogen in the first stage is 500, the temperature of the adsorption process is 25 ° C. The volumetric flow rate of the hydrogen stream to the second stage of the reactor is 1000, the temperature at the second stage is 50 ° C. The mercury content in the source hydrogen is 0.3 mg / m

sd

ten

00

sd

1C

The oxygen content in hydrogen before the reaction The mercury content in hydrogen after purification The degree of mercury removal The oxygen content in hydrogen after the reaction The degree of oxygen removal

Example 2. The volumetric feed rate of hydrogen in the first stage is 1000 h, the temperature of adsorption is 25 ° C. The volumetric flow rate of hydrogen in the second stage of the reactor is 1000, the reaction temperature is 50 ° C.

The mercury content in the source hydrogen is 0.3 mg / m

The oxygen content in the original hydrogen. 1.0% Mercury content in hydrogen after adsorption: Omg / m; Degree of mercury removal; 100% Oxygen content in hydrogen after the reaction is about vol. 0.08% Degree of Oxygen Removal 92%

From the above examples, it can be seen that the selected reagent — the spent Pd-containing catalyst K — PG performs deep complex purification of technical hydrogen from both oxygen and impurities of mercury vapor.

The method was also tested during long-term commercial operation of a two-stage 1 O reactor.

Example 3. Consumption of technical hydrogen in the reactor 450 l / h. Loading of the first stage of the reactor with a spent Pd-containing catalyst 650 ml. The volumetric flow rate of hydrogen in the first stage of the reactor is 692, the temperature in the first stage is equal to.

Pd catalyst loading in the second stage 450 ml. The volumetric flow rate of gas into the second stage of the reactor is 1000, the temperature in the second stage is equal to stage 7p .:

0

five

0

five

0

0.03 mg / m 94%

about. 0.12% 74%

The mercury content in the source hydrogen is 0.5 mg / m

The oxygen content in the original hydrogen. 0.47% Mercury content in hydrogen after adsorption Degree of mercury removal Oxygen content in hydrogen after reaction Degree of oxygen removal Example 4. The conditions of the test are the same as in the previous examples. The mercury content in the initial hydrogen I mg / m The oxygen content in the initial hydrogen is about. 1.51% Mercury content in hydrogen after adsorption Degree of mercury removal Oxygen content in hydrogen after reactivity Oxygen removal rate

Tests were carried out in the months and the effectiveness of the reagent was reversed.

In order to substantiate the materiality of the proposed parameters, experiments No. 5 and No. 6 were carried out.

Example 5. The volumetric feed rate of hydrogen is 2000. The temperature is 100 ° C. The oxygen content in the purified hydrogen is equal to about. 1.0%.

The oxygen content in hydrogen after the reaction is about. 0.076%.

The degree of oxygen removal is raviya 93%. The volumetric feed rate of hydrogen is 5000. The temperature is 70 ° C. The oxygen content in the original hydrogen is about. 1.0%.

The oxygen content in hydrogen after the reaction is about. 0.1%.

The degree of oxygen removal is 90%. The data on the purification efficiency are given in the table (adsorption is carried out at atmospheric pressure and 25 ° C, catalytic purification is carried out at atmospheric pressure and 70 ° C).

OMG / m 100%

about. 0.51% 75%

for two do not take off

1) volume flow rate of hydrogen, h

-five

1000

The degree of udshteni mercury,%

The degree of removal of oxygen,%

1000

5000

5000

100

50

90

1528542

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Claims (1)

The invention claims as a catalyst is spent The method of purification of hydrogen from impurities palladium containing catalyst CNG, and oxygen by reducing it during the in-process is carried out in two stages, with the presence of a palladium catalyst, the first-in the course of hydrogen is carried out at its  the fact that, in order to increase the ste-5, the space velocity is 500-1000, and in addition to cleaning and to provide an opportunity — at 25-100 ° C and the space velocity simultaneous purification from impurity of mercury, b1000-5000.