SU316468A1 - Getting salt hydroxylamine - Google Patents

Getting salt hydroxylamine

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Publication number
SU316468A1
SU316468A1 SU1197742A SU1197742A SU316468A1 SU 316468 A1 SU316468 A1 SU 316468A1 SU 1197742 A SU1197742 A SU 1197742A SU 1197742 A SU1197742 A SU 1197742A SU 316468 A1 SU316468 A1 SU 316468A1
Authority
SU
USSR - Soviet Union
Prior art keywords
metal
catalyst
hydroxylamine
platinum
liters
Prior art date
Application number
SU1197742A
Other languages
Russian (ru)
Inventor
Юли Томашевска Иностранцы Люци Матушевска
Народна Республика Польска
Publication of SU316468A1 publication Critical patent/SU316468A1/en

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Description

A known method of preparing a catalyst for obtaining a hydroxylamine salt is by converting a compound of a platinum group metal to a soluble state, followed by reduction in the presence of a carrier to a metal in two stages. In the first stage, the reduction to the bivalent state is carried out, for example, sulfoxylic acid derivatives, in the second stage, to form a metal with formic acid, hydrazine, formaldehyde, etc. The reduction is carried out at a pH of not more than 7.

In order to obtain a highly active catalyst and to simplify the process, it is proposed to reduce the compound of a platinum group metal to a metal in the presence of a carrier at minus 5 - plus 70 ° C, preferably approximately, in a dilute solution prepared from approximately 1 kg of platinum group metal, no less than than 300 liters of solution, preferably 600 liters.

The reduction of the metal compound of platinum metal is desirable to be carried out at a pH of more than 9. For reducing agents, solutions of formalin, hydrazine, formic acid, etc. can be used.

Example 1. To 9.9 kg of finely divided graphite, activated carbon or soot, 12 liters of an aqueous solution of H2PtCl6 containing 100 g of Pt are added. Received

the mixture is heated to 50-80 ° C. At this temperature, the mixture is continuously stirred for 4 hours, after which 3 l of 10% aqueous formaldehyde solution is added dropwise and 5 l of 48% -iHoro are poured.

aqueous solution at such a rate that the temperature of the mixture does not exceed. After adding the total amount of CPC, the mixture is diluted with 18.4 liters of water, stirred for 1 hour at normal temperature and 1 hour.

at 55 ° C. The catalyst is filtered, rinsed with water and dried in an atmosphere of air or oxygen.

The resulting catalyst is used in the synthesis of the hydroxylamine salt at 40 ° C. Catalyst activity approx 150 g

N0 / 2 platinum per hour at a selectivity of 90 -

99% (this means that 90-99% of the reacted nitric oxide forms hydroxylamine).

Example 2. The experiment is carried out similarly.

Example 1, but after filtration and washing, the product obtained is diluted with 50 liters of water, treated with hydrogen for 2 hours, then 50 liters of water containing 6 g of H2O2 is added. The catalyst is used in the preparation process. The catalyst exhibits high activity in the synthesis of hydroxylamine from nitric oxide and hydrogen in the presence of acid. This catalyst can be stored for a long time, it is characterized by very high activity at high selectivity, which allows to increase the yield of hydroxylamine salts per unit volume of the apparatus and at the same time reduce the amount of the deficient metal from the platinum group. The hydroxylamine salts formed in this way contain only small admixtures of ammonium salts. The proposed method of obtaining the catalyst is more commonly known, the raw materials for the process are cheap and affordable, as a result of which the synthesis of hydroxylamine becomes more economical. The subject matter of the invention is 1. A method for preparing a catalyst for producing a hydroxylamine salt by converting a platinum-group metal compound to soluble state and then reducing it in the presence of a carrier to a metal, characterized in that, in order to simplify the process and to obtain a highly active catalyst, The platinum group is carried out at minus 5 - PLEO: C 70 ° C, preferably at a temperature of about 30 ° C, in a dilute solution prepared at the rate of about 1 kg of platinum metal Rupp not less than 300 liters of solution, preferably 600 liters of solution. 2. The method according to claim 1, characterized in that the reduction of the compound of the platinum group metal is carried out at a pH of more than 9. 3. The method according to mon. 1 and 2, characterized in that the reduced-slip catalyst is subjected to the action of an oxidizing agent, such as hydrogen peroxide, oxygen, etc.

SU1197742A Getting salt hydroxylamine SU316468A1 (en)

Publications (1)

Publication Number Publication Date
SU316468A1 true SU316468A1 (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4992252A (en) * 1987-09-22 1991-02-12 Sumitomo Chemical Company, Limited Method for production of hydroxylammonium salt
US5120699A (en) * 1990-07-18 1992-06-09 Basf Aktiengesellschaft Platinum-on-graphite catalysts and the use thereof
US5155081A (en) * 1990-07-18 1992-10-13 Basf Aktiengesellschaft Platinum-on-graphite catalysts

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4992252A (en) * 1987-09-22 1991-02-12 Sumitomo Chemical Company, Limited Method for production of hydroxylammonium salt
US5120699A (en) * 1990-07-18 1992-06-09 Basf Aktiengesellschaft Platinum-on-graphite catalysts and the use thereof
US5155081A (en) * 1990-07-18 1992-10-13 Basf Aktiengesellschaft Platinum-on-graphite catalysts

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