GB/T 37359-2019 English PDF (GBT37359-2019)

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GB/T 37359-2019: Test method of activity for palladium carbon catalysts
GB/T 37359-2019
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.99
G 74
Test method of activity for palladium carbon catalysts
ISSUED ON: MARCH 25, 2019
IMPLEMENTED ON: FEBRUARY 01, 2020
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Principle ... 4 
4 Reagents or materials ... 4 
5 Test device ... 5 
6 Sample ... 6 
7 Test procedures ... 7 
8 Test data processing ... 8 
Test method of activity for palladium carbon catalysts
1 Scope
This Standard specifies the test method of activity for palladium carbon
catalysts.
This Standard applies to palladium carbon catalysts of hydrogenation reduction
reactions for petrochemical industry, pharmaceutical intermediates, electronics
industry, perfume industry, dye industry and other fine chemicals, which takes
wood powdered activated carbon as the carrier and palladium as the main
active component.
2 Normative references
The following documents are indispensable for the application of this document.
For dated references, only the dated version applies to this document. For
undated references, the latest edition (including all amendments) applies to this
document.
GB/T 6679, General rules for sampling solid chemical products
GB/T 6682, Water for analytical laboratory use. Specification and test
methods
3 Principle
The N-benzylaniline in the raw material, under certain temperature and
pressure and the action of a palladium carbon catalysts, reacts with hydrogen
to generate aniline and toluene. The chemical reaction formula is as follows:
Use a gas chromatograph to determine the mass fraction of N-benzylaniline
before and after the reaction; calculate the conversion rate of N-benzylaniline,
to characterize the activity of the catalyst.
4 Reagents or materials
4.1 N-Benzylaniline: purity greater than 99.0%.
Weigh 0.010 0 g of the catalyst sample corresponding to palladium; accurate to
0.000 1 g; put aside for use.
7 Test procedures
Warning -- The test materials and reagents which are involved in this
Standard have toxic, flammable, and explosive hazards to human health
and safety. System leakage shall be strictly prevented; open flames are
strictly forbidden on the site; preventive facilities such as necessary fire
extinguishing equipment and exhaust equipment shall be equipped; it is
strictly forbidden to carry out disassembly operation of autoclave under
pressure. This Standard does not reveal all possible safety issues; users
shall use it strictly in accordance with relevant regulations, and have the
responsibility to take appropriate safety and health measures.
7.1 Filling of the reactor
Add 30.0 g of N-benzylaniline, 150 mL of ethanol, 1.0 mL of formic acid, and
catalyst samples (see 6.3) to the clean and dry reactor in order; cover the kettle
lid; tighten the nuts evenly; then, connect it to the system.
7.2 Leakage test
Open the nitrogen valve; introduce nitrogen into the system; boost the system
to 0.50 MPa; close the inlet and outlet valves of the system. If the pressure drop
is less than 0.05 MPa within 30 min, the system is considered to be sealed.
Open the system outlet valve to reduce the pressure of the system to normal
pressure; insert the temperature measuring thermocouple into the thermowell.
7.3 Gas replacement and activity determination
Use nitrogen to replace the system for 3 times; then, exhaust and reduce the
pressure to normal pressure. Switch to hydrogen and replace for 3 times; then,
exhaust and reduce the pressure to normal pressure. Warm and heat the
reactor. When the temperature of the reactor is raised to 50°C, increase the
system pressure to 0.50 MPa. Control and maintain the reactor pressure at 0.50
MPa, the temperature at 50°C, and the stirring speed at 900 r/min. After 20
minutes, end the test.
7.4 Power-off
Turn off the hydrogen and turn on the cooling water; after the temperature of
the reactor drops to below 40°C, release the pressure. Use nitrogen to replace
the system for 3 times; perform sampling and analysis; use deionized water to
clean the reactor body.