Method for producing industrial grade superior ammonium sulfate through coked coarse ammonium sulfate dilution crystallization

A technology of dissolution crystallization and crude ammonium sulfate, which is applied in the field of product ammonium sulfate, can solve the problems of easy crystal sinking, prolonged crystallization time, high solubility, etc., and achieve the effects of slowing down the growth rate, improving the color level, and reducing the content of impurities

Inactive Publication Date: 2014-01-08
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, regardless of evaporative crystallization or cooling crystallization, crystal scale is easy to form on heat exchange surfaces such as coils or jackets, which significantly reduces heat transfer efficiency, makes it difficult to control the evaporation rate or cooling rate, and prolongs the crystallization time, resulting in a particle size distribution of crystallized products. Inhomogeneity, low production efficiency
Moreover, for the evaporative crystallization process, the solid-liquid suspension density in the crystallizer is getting higher and higher, the crystal-liquid mixing is uneven, the crystal is easy to sink to the bottom, and the friction and collision between the crystals and between the crystal and the stirring paddle causes the crystal to break during the crystallization process. Seriously, this will also aggravate the uneven particle size distribution of crystallized products
In addition, ammonium sulfate has a high solubility in water (0°C, 70g / 100g water). Regardless of evaporation crystallization or cooling crystallization, there will still be a large amount of uncrystallized ammonium sulfate in the mother liquor at the end of crystallization, resulting in low production capacity per unit volume crystallizer.

Method used

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  • Method for producing industrial grade superior ammonium sulfate through coked coarse ammonium sulfate dilution crystallization

Examples

Experimental program
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Effect test

Embodiment 1

[0035] A method for producing industrial-grade high-quality ammonium sulfate by dissolution and crystallization of coking crude ammonium sulfate, the specific steps of which are:

[0036] Step 1. Under the condition of rotating speed of 200-300r / min, first prepare a coking crude ammonium sulfate aqueous solution with a concentration of 40-45wt%; then use NaOH to adjust the pH of the coking crude ammonium sulfate solution to 7-8; adding activated carbon accounting for 1-3wt% of the coking crude ammonium sulfate into the aqueous solution, insulated and stirring for 0.5-1 hour, and then insulated and filtered to obtain the coking crude ammonium sulfate crystallization mother liquor;

[0037] Step 2. Under the condition of rotating speed of 200-300r / min, first add an acid regulator to the coking crude ammonium sulfate crystallization mother liquor prepared in step 1 to make the pH of the mother liquor = 5~6; then add crystal habit modification to the mother liquor Agent and seed c...

Embodiment 2

[0042] A method for producing industrial-grade high-quality ammonium sulfate by dissolution and crystallization of coking crude ammonium sulfate, the specific steps of which are:

[0043] Step 1. Under the condition of rotating speed of 300-400r / min, first prepare a coking crude ammonium sulfate aqueous solution with a concentration of 43-48wt%; then use NaOH to adjust the pH of the coking crude ammonium sulfate solution to 8-9; adding activated carbon accounting for 2-4wt% of the coking crude ammonium sulfate into the aqueous solution, incubating and stirring for 0.5-1 h, and then insulated and filtering to obtain the coking crude ammonium sulfate crystallization mother liquor;

[0044] Step 2. Under the condition of rotating speed of 300-400r / min, first add an acid regulator to the coking crude ammonium sulfate crystallization mother liquor prepared in step 1 to make the pH of the mother liquor = 6~7; then add crystal habit modification to the mother liquor Agent and seed cr...

Embodiment 3

[0049] A method for producing industrial-grade high-quality ammonium sulfate by dissolution and crystallization of coking crude ammonium sulfate, the specific steps of which are:

[0050] Step 1. Under the condition of rotating speed of 400-500r / min, firstly prepare a coking crude ammonium sulfate aqueous solution with a concentration of 45-50wt%; then use NaOH to adjust the pH of the coking crude ammonium sulfate solution to 8-9; adding activated carbon accounting for 3-5wt% of the coking crude ammonium sulfate into the aqueous solution, incubating and stirring for 0.5-1 hour, and then insulated and filtering to obtain the coking crude ammonium sulfate crystallization mother liquor;

[0051] Step 2. Under the condition of rotating speed of 400-500r / min, first add an acid regulator to the coking crude ammonium sulfate crystallization mother liquor prepared in step 1 to make the pH of the mother liquor = 6~7; then add crystal habit modification to the mother liquor Agent and se...

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Abstract

The invention particularly relates to a method for producing industrial grade superior ammonium sulfate through coked coarse ammonium sulfate dilution crystallization. According to the technical scheme, the method comprises the steps that the pH value of a coked coarse ammonium sulfate aqueous solution is adjusted through NaOH, activated carbon is further added, and the aqueous solution is filtered, so that a coked coarse ammonium sulfate crystallization mother solution is obtained; an acidity adjusting agent, a crystal habit modification agent and seed crystals are added to the mother solution, crystal is cultivated, and therefore suspended turbid crystal mush is prepared; finally, eluent is added to suspended turbid crystal mush flow, dilution crystallization is conducted, ammonium sulfate crystals are prepared through filtration and drying, the particle size distribution of a crystal product is concentrated, the surface is smooth, the purity is high, the liquidity is good, and the standard of an industrial grade superior product can be met. The particle size and the addition quantity of the seed crystals are changed so that the average particle size and the particle size distribution of the ammonium sulfate crystal product can be adjusted and controlled in the process of crystallization. The method for producing the industrial grade superior ammonium sulfate through coked coarse ammonium sulfate dilution crystallization has the advantages that the production cost is low, the production cycle is short, the average particle size is controllable, the particle size distribution is concentrated, one-way crystallization yield is high (no less than 95%), and the quality of the product is high.

Description

technical field [0001] The invention belongs to the technical field of industrial crystallization, and in particular relates to a method for producing industrial-grade high-quality ammonium sulfate by dissolution and crystallization of coking crude ammonium sulfate. Background technique [0002] Coking ammonium sulfate is a large industrial by-product of coke oven gas purification. A JN60-60 type 2×65 hole 7m 63 coke oven with an annual output of 2 million tons of coke can reach 30,000 t / a of ammonium sulfate. Since 1993, my country's coke output has been ranked first in the world, and it exceeded 400 million tons in 2011, so the output of domestic coking ammonium sulfate is huge. Ammonium sulfate is an important nitrogen fertilizer, and it can also be used as printing and dyeing agent, food catalyst, buffering agent, leather deliming agent and so on in industry. [0003] At present, most coking plants in China use the saturator method to produce ammonium sulfate. Coking ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01C1/24C01C1/248
Inventor 张春桃刘帮禹王鑫王海蓉
Owner WUHAN UNIV OF SCI & TECH
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