GB/T 37360-2019 English PDF (GBT37360-2019)

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GB/T 37360-2019: Test method of activity for rhodium carbon catalysts
GB/T 37360-2019
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.99
G 74
Test method of activity for rhodium 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 Determination procedures ... 6 
8 Test data processing ... 8 
Test method of activity for rhodium carbon catalysts
1 Scope
This Standard specifies the test method of activity for rhodium carbon catalysts.
This Standard applies to rhodium carbon catalysts for hydrogenation reduction
of aromatic rings, heterocyclic rings, nitro, nitriles, fatty carboxylic acids and
other fine chemicals.
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
O-chloronitrobenzene in the raw material reacts with hydrogen to form o-
chloroaniline and water under the action of rhodium carbon catalyst. Its
chemical reaction formula is as follows:
Use a gas chromatograph to determine the mass fraction of o-
chloronitrobenzene before and after the reaction; calculate the conversion rate
of o-chloronitrobenzene, to characterize the activity of the catalyst.
4 Reagents or materials
4.1 O-chloronitrobenzene: purity greater than 99.0%.
4.2 Methanol: analytical reagent.
4.3 Deionized water: grade-II water which is specified in GB/T 6682.
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 reactor 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 o-chloronitrobenzene, 150 mL of methanol, 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 1.00 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 75°C, increase the
system pressure to 1.00 MPa. Control and maintain the reactor pressure at 1.00
MPa, the temperature at 75°C, and the stirring speed at 1 000 r/min. After 1
hour, 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.
7.5 Determination of o-chloronitrobenzene mass fraction
7.5.1 Chromatograph operating conditions
Chromatographic column: DB-1 (30 m × 0.25 mm × 0.25 μm).
Nitrogen flow: 30.0 mL/min.
Hydrogen flow: 40.0 mL/min.