Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of acetone thiosemicarbazone and the prepared acetone thiosemicarbazone

A technology of acetone thiosemicarbazone and acetone is applied in the fields of medicine and pesticide compounds, which can solve the problems of low yield and low purity of finished products, and achieve the effect of high income

Active Publication Date: 2019-03-12
宁夏顺邦达新材料有限公司
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the technical defects of low yield and low purity of the finished product in the existing method for preparing acetone thiosemicarbazone, the present invention provides a preparation method of acetone thiosemicarbazone and the product obtained by the preparation method, realizing the The production rate and finished product are significantly improved, and the preparation process has no corrosion, and the by-products can be recycled and reused.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of acetone thiosemicarbazone and the prepared acetone thiosemicarbazone
  • Preparation method of acetone thiosemicarbazone and the prepared acetone thiosemicarbazone
  • Preparation method of acetone thiosemicarbazone and the prepared acetone thiosemicarbazone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment one: the preparation method of a kind of acetone thiosemicarbazone disclosed by the present invention, comprises the following steps, (1) puts the raw material prepared in reactor, and raw material comprises water, hydrazine hydrate, ammonium thiocyanate;

[0022] (2) Heating causes the raw materials to undergo a chemical reaction, and the chemical reaction equation is as follows:

[0023] (N 2 h 4 )H 2 O+NH 4 SCN→N 2 h 4 HSCN+NH 3 +H 2 O;

[0024] (3) When the temperature of reaction rose to 40°C, the reactor was evacuated to discharge the ammonia generated by the reaction;

[0025] (4) The reaction kettle is cooled, and when the temperature is lowered to 30° C., acetone is added in the reaction kettle;

[0026] (5) Acetone reacts exothermicly with hydrazine thiocyanate, and the chemical reaction equation is as follows:

[0027] N 2 h 4 HSCN+(CH 3 ) 2 CO——(CH 3 ) 2 CNNHCSNH 3 +H 2 o

[0028] (6) When the reaction temperature reaches 50° C....

Embodiment 2

[0032] Embodiment two: the preparation method of a kind of acetone thiosemicarbazone disclosed by the present invention, comprises the following steps, (1) puts the raw material prepared in the reactor, and raw material comprises water, hydrazine hydrate, ammonium thiocyanate;

[0033] (2) Heating causes the raw materials to undergo a chemical reaction, and the chemical reaction equation is as follows:

[0034] (N 2 h 4 )H 2 O+NH 4 SCN→N 2 h 4 HSCN+NH 3 +H 2 O;

[0035] (3) When the temperature of reaction rose to 50°C, the reactor was evacuated to discharge the ammonia generated by the reaction;

[0036] (4) The reactor is cooled, and when the temperature is lowered to 15° C., acetone is added into the reactor;

[0037] (5) Acetone reacts exothermicly with hydrazine thiocyanate, and the chemical reaction equation is as follows:

[0038] N 2 h 4 HSCN+(CH 3 ) 2 CO——(CH 3 ) 2 CNNHCSNH 3 +H 2 o

[0039] (6) When the reaction temperature reaches 80° C., a reflux...

Embodiment 3

[0045] Embodiment three: the preparation method of a kind of acetone thiosemicarbazone disclosed by the present invention, comprises the following steps, (1) puts the raw material prepared in the reactor, and raw material comprises water, hydrazine hydrate, ammonium thiocyanate;

[0046] (2) Heating causes the raw materials to undergo a chemical reaction, and the chemical reaction equation is as follows:

[0047] (N 2 h 4 )H 2 O+NH 4 SCN→N 2 h 4 HSCN+NH 3 +H 2 O;

[0048] (3) When the temperature of reaction rose to 45°C, the reactor was evacuated to discharge the ammonia generated by the reaction;

[0049] (4) The reaction kettle is cooled, and when the temperature is lowered to 35° C., acetone is added in the reaction kettle;

[0050] (5) Acetone reacts exothermicly with hydrazine thiocyanate, and the chemical reaction equation is as follows:

[0051] N 2 h 4 HSCN+(CH 3 ) 2 CO——(CH 3 ) 2 CNNHCSNH 3 +H 2 o

[0052] (6) When the reaction temperature reaches ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method of acetone thiosemicarbazide. The preparation method comprises (1) putting raw materials for preparation into a reactor, (2) heating the raw materials to cause the chemical reaction, (3) when the reaction temperature is increased to 40 to 50 DEG C, carrying out vacuum pumping on the reactor and discharging the produced ammonia gas, (4) cooling the reactor to 30 DEG C and adding acetone into the reactor, (5) carrying out an exothermic reaction process on acetone and thiocyanate, and (6) when the reaction temperature is 50 to 80 DEG C, adding the reaction product into a reflux device to prevent the liquid evaporation so that acetone thiosemicarbazone is obtained. The preparation method has advantages of final product yield higher than 90% and product purity of 99%. The ingredients in the novel raw materials do not corrode the equipment. The by-product ammonia gas can be collected and processed to form ammonium hydroxide for recycling. The preparation method has a high yield and does not produce pressure on equipment and environment.

Description

technical field [0001] The invention relates to the technical field of medicine and pesticide compounds, in particular to a preparation method of acetone thiosemicarbazone and the acetone thiosemicarbazone obtained through the method. Background technique [0002] Acetone thiosemicarbazone is an intermediate of pharmaceuticals and pesticides, and can also be used as a terminator for terminating the polymerization reaction during the polymerization of PVC. The industrial production method of domestic manufacturers is the atmospheric pressure sulfuric acid method. The steps are the reaction of hydrazine hydrate and sulfuric acid to produce hydrazine sulfate. Thiosemicarbazide. [0003] This process route has the disadvantages of low yield (75-85%), low purity of finished product (about 95%), great corrosion of equipment by sulfuric acid, and difficult handling of by-product ammonium sulfate. The equation for this reaction is as follows: [0004] Contents of the inventio...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C337/08C01C3/20
CPCC01C3/20C07C337/08
Inventor 朱国成
Owner 宁夏顺邦达新材料有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com