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Method for reusing by-product ammonia gas produced in production process of cationic blue X-BL

A technology of X-BL and production process, which is applied in the direction of organic chemistry, can solve the problems of waste of resources and increase of enterprise costs, and achieve the effects of reducing production energy consumption, easy operation, good economic and environmental benefits

Inactive Publication Date: 2019-09-13
HENAN CHEM IND RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of preparing thiosemicarbazide by using the ammonia exhaust method directly enters the tail gas absorption tower and treats it as waste liquid, which not only causes waste of resources, but also increases the cost of the enterprise.
[0004] And in the preparation method of 2-amino-1,3,4-thiadiazole, usually raw material thiosemicarbazide, hydrochloric acid and formic acid are heated and refluxed in the reactor, cooled, neutralized with sodium hydroxide aqueous solution, adjusted pH to 8-9, filtered to obtain the product, and the use of ammonia water (ammonia) to adjust the pH has not been reported

Method used

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  • Method for reusing by-product ammonia gas produced in production process of cationic blue X-BL
  • Method for reusing by-product ammonia gas produced in production process of cationic blue X-BL

Examples

Experimental program
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Effect test

Embodiment 1

[0018] In the method for the present invention, the cationic blue X-BL production process includes the preparation of intermediate thiosemicarbazide and intermediate 2-amino-1,3,4-thiadiazole; the specific method steps are as follows:

[0019] a. Add the raw materials ammonium thiocyanate and hydrazine hydrate into the reactor I, start heating and stirring, when the temperature of the reactor rises to 82 o Open the air pump during C; when the reactor II is not neutralized, open the valve II connecting the reactor I and the ammonia absorption tower, and pass the generated by-product ammonia into the ammonia absorption tower for subsequent use;

[0020] b. Put 920 g of thiosemicarbazide, 800 mL of hydrochloric acid and 600 g of formic acid into the reaction kettle II, turn on the heating and heat up to 80 o C, after the solid is completely dissolved, continue to heat up to 110 o C, reflux for 4.5 h, after cooling, close the valve II connecting the reactor I and the ammonia abso...

Embodiment 2

[0024] In the method for the present invention, the cationic blue X-BL production process includes the preparation of intermediate thiosemicarbazide and intermediate 2-amino-1,3,4-thiadiazole; the specific method steps are as follows:

[0025] a. Add the raw materials ammonium thiocyanate and hydrazine hydrate into the reactor I, start heating and stirring, when the temperature of the reactor rises to 80 o Open the air pump during C; when the reactor II is not neutralized, open the valve II connecting the reactor I and the ammonia absorption tower, and pass the generated by-product ammonia into the ammonia absorption tower for subsequent use;

[0026] b. Put 920 g of thiosemicarbazide, 600 mL of hydrochloric acid and 600 g of formic acid into the reaction kettle II, turn on the heating and heat up to 80 o C, after the solid is completely dissolved, continue to heat up to 105 o C, reflux for 4.5 h, after cooling, close the valve II connecting the reactor I and the ammonia abso...

Embodiment 3

[0030] In the method of the present invention, the cationic blue X-BL production process includes the preparation of intermediate thiosemicarbazide and intermediate 2-amino-1,3,4-thiadiazole; the specific method steps are as follows:

[0031] a. Add the raw materials ammonium thiocyanate and hydrazine hydrate into the reactor I, start heating and stirring, when the temperature of the reactor rises to 85 o Open the air pump during C; when the reactor II is not neutralized, open the valve II connecting the reactor I and the ammonia absorption tower, and pass the generated by-product ammonia into the ammonia absorption tower for subsequent use;

[0032] b. Put 1002 g of thiosemicarbazide, 800 mL of hydrochloric acid and 600 g of formic acid into the reaction kettle II, turn on the heating and heat up to 85 o C, after the solid is completely dissolved, continue to heat up to 115 o C, reflux for 4.5 h, after cooling, close the valve II connecting the reactor I and the ammonia abso...

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Abstract

The invention provides a method for reusing the by-product ammonia gas produced in production process of cationic blue X-BL. The production process of cationic blue X-BL comprises the preparation of the intermediate thiosemicarbazide and the intermediate 2-amino-1,3,4-thiadiazole. The method comprises the following concrete steps: applying a great amount of by-produced ammonia gas generated in a reaction for preparing thiosemicarbazide via an ammonia discharging process to a reaction vessel I, and when a reaction vessel II does not use ammonia gas, starting an air pump to bring the by-producedammonia gas to an ammonia absorption tower for generation of ammonia water which may be used as alkaline liquid for adjusting a pH value in the reaction vessel II; after completion of heating refluxof raw materials consisting of thiosemicarbazide, formic acid and hydrochloric acid in the reaction vessel II, opening a corresponding valve, introducing the by-produced ammonia gas or adding the ammonia water in the ammonia absorption tower and adjusting a pH value to 8-9; and carrying out cooling to obtain high-purity 2-amino-1,3,4-thiadiazole. The method of the invention effectively utilizes the by-product ammonia gas produced in production process of cationic blue X-BL, reduces the emission pollution of ammonia gas, reuses existing resources, has high product yield and is simple in operation.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a recycling method for by-produced ammonia in the production process of cationic blue-born X-BL. Background technique [0002] Cationic blue is a blue-green powder, easily soluble in water and turns blue. The shade of dyeing remains unchanged at high temperature, and the color changes slightly when it encounters copper and iron ions. Mainly used for acrylic dyeing, it can dye acrylic loose fibers, fiber strips, acrylic wool, knitted fleece, knitted fabrics, blankets, etc. It can also be used for direct printing of the above fabrics; it is suitable for dyeing brighter light blue, usually with cationic Yellow X-6G and cationic red X-GRL form the three primary colors, which can be blended and dyed in various light to dark shades, from bright blue with reddish light to rich navy blue. It can also be used for the dyeing of modified polyester, but it is generall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D285/135C07C337/06
CPCC07D285/135C07C337/06
Inventor 程伟琴霍二福王柏楠孙耀峰李迎春陈蔚刘仁义刘晨义冯明杨帅鲁鹏王毅楠王延花陈珂高青环张志岩吴泽鑫韩娟付政辉黄蓓郭歌杜玉杰王大陆郭骏李晓琼刘沛敬常书浩王现洋王宏力
Owner HENAN CHEM IND RES INST
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