Process for preparing hydroxylamine salt by continuous hydrolysis of oxime

The technology of a hydroxylamine salt and a process is applied in the field of a new process for the preparation of hydroxylamine salt, can solve the problems of residual oxime in hydrolyzate, catalyst deactivation, oxime loss and the like, and achieves the advantages of simple post-treatment process, simple synthesis method and high product selectivity. Effect

Active Publication Date: 2020-06-26
CHEM TECH ACAD OF SHANDONG PROVINCE
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Although the occurrence of side reactions is reduced, the hydrolysis temperature is low, which inhibits the hydrolysis balance, and will cause a large amount of unreacted oxime to remain in the hydrolyzed solution. The decompression dehydration of the hydrolyzed solution will cause a large amount of oxime loss, and the product needs to be refined by ethanol , the introduction of organic solvents
Some patents also use low-temperature hydrolysis, adding a titanium-silicon molecular sieve catalyst to catalyze the hydrolysis, the interstitial hydrolysis time is longer, the strong acid system is likely to cause catalyst deactivation, and there are problems with catalyst separation, activation and regeneration
[0005] The above hydrolysis methods have problems such as low selectivity, refined products, many by-products, and serious environmental pollution.

Method used

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  • Process for preparing hydroxylamine salt by continuous hydrolysis of oxime

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Effect test

Embodiment 1

[0036] A process for preparing hydroxylamine salt by continuous hydrolysis of oxime, using oxime and acid as raw materials, continuous production, and realizing the process through the following devices;

[0037] The concrete structure of described device is as follows:

[0038] The oxime source 1 and the acid source 2 are connected to the static mixer 3, the top of the static mixer 3 is connected to the preheater 4, the preheater 4 is connected to the external heat exchanger 5 of the hydrolysis kettle, and the external heat exchanger 5 of the hydrolysis kettle is connected to the top of the hydrolysis kettle 6, The top of the hydrolysis kettle 6 is connected to the condenser 8, the condenser 8 is connected to the liquid separator 9, and the liquid separator 9 is connected to the ketone collecting device;

[0039] The bottom of the hydrolysis kettle 6 is connected to the heat exchanger 10, the heat exchanger 10 is connected to the top of the decolorization kettle 11, the botto...

Embodiment 2

[0047] A new process for preparing hydroxylamine salt by continuous hydrolysis of oxime. Oxime 1 and acid 2 are continuously fed into static mixer 3 at a ratio of 1.1:1, and the acid and oxime are fully mixed to obtain a hydrolyzed stock solution; the hydrolyzed stock solution is preheated by a preheater 4 to 50°C; the preheated hydrolysis stock solution continuously enters the inlet of the external heat exchanger 5 of the hydrolysis kettle, and starts hydrolysis for 3 minutes after being heated to 65°C, and the ketone and hydroxylamine obtained by hydrolysis are separated above the hydrolysis kettle 6, and the hydrolyz The upper connection port is a Venturi-type injector 7; the rising steam of the hydrolysis kettle brings the vaporized ketone into the condenser 8, and the condensate is separated by liquid separator 9, and the water phase after liquid separation is returned to the hydrolysis kettle for separation. The ketone obtained from the solution is used for the oximation ...

Embodiment 3

[0049] Butanone oxime and acid are continuously fed into the static mixer at a ratio of 1.3:1 to configure the hydrolyzate. The outlet of the static mixer is connected to the inlet of the heat exchanger outside the hydrolysis kettle, and the feed rate is maintained at 200kg / h. Heater continuous hydrolysis, adjust circulation pump to 12.5m 3 / h, while the production liquid flow rate is 200kg / h, the temperature at the bottom of the tank is 106°C, and the azeotrope of ketone and water is produced at the top of the tower. The extracted hydrolyzate is decolorized with activated carbon for about 30 minutes, and the decolorization temperature is 60°C. The decolorization liquid is dehydrated by a concentrated evaporation device, the dehydration temperature is less than 80°C, and the pressure is ≥-0.095MPa. After the concentrated solution is cooled by a continuous cooling crystallizer, the product is centrifugally dried, and the product purity reaches 99.3%.

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Abstract

The invention belongs to the field of hydroxylamine salt preparation, and particularly relates to a continuous preparation process of a hydroxylamine salt. According to the process, ketoxime and hydrochloric acid (sulfuric acid) are used as raw materials and are subjected to continuous hydrolysis to prepare a hydroxylamine salt; and the process comprises: preparing a hydrolysis stock solution fromketoxime and hydrochloric acid (sulfuric acid), pumping the hydrolysis stock solution into a hydrolysis kettle, continuously producing a hydrolysis completion liquid from the hydrolysis kettle, decolorizing the hydrolysis completion liquid by active carbon, feeding into a concentration device, continuously cooling and crystallizing the concentrated completion liquid, feeding into a centrifugal machine, returning centrifugal mother liquor to a decolorizing liquid tank, and drying the centrifugal product to obtain a finished product hydroxylamine salt. According to the hydrolysis process, continuous operation of hydrolysis, decoloration and crystallization is realized, the equipment utilization rate is greatly improved, the hydrolysis efficiency is improved, the retention time of a hydrolysis stock solution is short, and excessive side reactions are avoided. The product purity is high, the superior product requirements are met, and the cost can be effectively reduced.

Description

technical field [0001] The invention belongs to the field of preparation of hydroxylamine salts, and in particular relates to a new preparation process of hydroxylamine salts. Background technique [0002] As an important chemical raw material, hydroxylamine salt is mainly used as a reducing agent and imaging agent. It is mainly used to prepare oximes in organic synthesis, and is also used to synthesize anticancer drugs (hydroxyurea), sulfa drugs (sulfamethoxazole) and Raw material of pesticide (methomyl). It is used as a depolarizer in electroanalysis and as a non-coloring short-term stopper in the synthetic rubber industry. The pharmaceutical industry is used as an intermediate of sulfamethoxazole. Synthetic dye industry is used as isatin intermediate preparation. In the oil industry, it is used as an anti-aging agent and antioxidant for fatty acids and soaps. In analytical chemistry, it is used as a reducing agent for the analysis of formaldehyde, furfural, camphor an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/14
CPCC01B21/1409C01B21/1472C01P2006/80Y02P20/10
Inventor 岳涛卢福军杨旭王达彤赵相柱冯维春
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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