CN1052455C

CN1052455C - Method for catalytic prodn. of potassium sulfate using potassium hydroxide

Info

Publication number: CN1052455C
Application number: CN97125304A
Authority: CN
Inventors: 何永汉; 何滨生; 何柳静
Original assignee: 何永汉
Priority date: 1997-12-03
Filing date: 1997-12-03
Publication date: 2000-05-17
Anticipated expiration: 2017-12-03
Also published as: CN1184778A

Abstract

The present invention relates to a method for producing potassium sulfate by taking potassium chloride and ammonium sulfate as principal raw materials. Ammonium sulfate is dissolved in hot water to obtain saturated solution, and then potassium chloride and potassium hydroxide are added to enable separated potassium sulfate to be crystallized; after potassium sulfate is obtained by centrifugal separation, ammonium bicarbonate is added in the solution, and then potassium sulfate is separated out; the clear solution is cooled to 5 to 15 DEG C, and ammonium chloride crystals can be obtained. The mother solution after centrifugal separation is cyclically used again. The method enables the reaction time to be shortened by 1/3, the purity of the potassium sulfate is high, and environmental pollution can not be caused.

Description

Potassium hydroxide catalysed is produced the method for vitriolate of tartar

The present invention relates to a kind of is that main raw material uses potassium hydroxide catalysed to produce the method for vitriolate of tartar with Repone K and ammonium sulfate.

The method with Repone K and ammonium sulfate production vitriolate of tartar of open source literature report is many at present, these methods respectively have characteristics, but some complex manufacturing are arranged, facility investment is big, the energy consumption height, apply and acquire a certain degree of difficulty, the method of a kind of ammonium sulfate and Repone K circulation PRODUCING POTASSIUM SULFATE BY DOUBLE DECOMPOSITION is disclosed as Chinese patent 93110467, it is in containing the aqueous solution of ammonium sulfate, add Repone K, refrigerated separation gets thick product and mother liquor I, thick product is added potassium chloride solution carries out aftertreatment, separate mother liquor III and wet product, drying gets vitriolate of tartar, mother liquor I is through concentrating, cold analysis, separate mother liquor II and ammonium chloride, mother liquor II, III recycles after mixing; Chinese patent 93103865 also discloses a kind of method of producing vitriolate of tartar by ammonium sulfate and Repone K, it is that ammonium sulfate, Repone K, ammonium mother liquor, potassium washing lotion and the reaction of cationic amine compound are made thick vitriolate of tartar and clear liquor, clear liquor obtains ammonium chloride potassium and ammonium mother liquor through refrigerated separation, and thick vitriolate of tartar and Klorvess Liquid obtain vitriolate of tartar and potassium washing lotion by proportioning (weight) reaction.Above-mentioned two kinds of methods of producing vitriolate of tartar with Repone K and ammonium sulfate are complicated, the bad grasp of process, sepn process is slow, yield is not high yet, second method also needs to add the higher cationic amine compound of cost, effect is also bad, thereby the method for at present directly producing vitriolate of tartar with Repone K and ammonium sulfate also fails to find cost low effective operational path.

The purpose of this invention is to provide and a kind ofly can overcome the deficiencies in the prior art part, have that method is simple, energy consumption is low, a production method of good product quality, vitriolate of tartar free from environmental pollution.

Production method feature of the present invention is to use hot water dissolving's ammonium sulfate of 65-90 ℃ earlier, obtain saturated ammonium sulphate solution, add the Repone K saturated aqueous solution by stoichiometric ratio then, add catalyzer potassium hydroxide again, be cooled to 50-60 ℃ after solution mixed, promptly separate out the vitriolate of tartar crystallization, obtain potassium product with the whizzer separation, the amount that stays Repone K according to solution after separating adds the bicarbonate of ammonia saturated aqueous solution again by stoichiometric ratio, mix, keep 50-60 ℃, separate out vitriolate of tartar for the second time, after centrifugation goes out solid sulphuric acid potassium, the clear liquid that leaches is cooled to 5-15 ℃, separates out ammonium chloride crystals, after the centrifugation, mother liquor adds saturated ammonium sulphate, Repone K and catalyzer, cyclic production once more.

The adding of catalyzer potassium hydroxide has two effects, the one, the pH value of control solution, make the water salt phasor of ammonium sulfate-Repone K-potassium hydroxide reach suitable potential of hydrogen that vitriolate of tartar generates and be issued to the maximum value (peak concentration) of product in suitable temperature, the 2nd, add Partial K ⁺, make reaction towards generation, K ₂SO ₄Direction transform, its add-on is generally the 5-30 ‰ of ammonium sulfate and Repone K saturated aqueous solution gross weight.

The present invention compared with the prior art, its substantive distinguishing features and obvious improvement are:

1. the use potassium hydroxide catalyst can make the reaction times shorten more than 1/3, and the production cycle is shortened greatly.

2. the potassium product quality is good, and purity can reach more than 98%, and the transformation efficiency of Repone K reaches more than 90%.

3. production technique is simple, and processing ease does not need complex apparatus, and not only being fit to original ammonium sulfate factory increases small number of devices production, also is fit to carbon ammonium factory and transforms and produce and the new composite fertilizer factory that builds produces.

4. do not have waste gas, waste residue, contaminated wastewater, do not influence surrounding environment, do not influence the healthy of millworker.

Below be embodiments of the invention:

Embodiment one, in stainless steel interlayer container, add clear water, with being steam heated to 85 ℃, pour the solid sulphuric acid ammonium solution into, until saturated, add saturated potassium chloride solution then and add 10 ‰ KOH solid, stir, be cooled to 55 ℃ by the total liquid measure of every 1000kg, promptly separated out the vitriolate of tartar crystallization in 20-30 minute, it is centrifugal that the solution filtration is drawn to whizzer, obtains solid sulphuric acid potassium, and the clear liquid after filter is sour and centrifugal adds the bicarbonate of ammonia saturated aqueous solution again, second separates out vitriolate of tartar, after centrifugation goes out solid sulphuric acid potassium, filtrate is cooled to 10 ℃, promptly separates out ammonium chloride crystals, same spline filter, centrifugation goes out solid ammonium chloride, and filtrate and centrifugal clear liquid add saturated ammonium sulphate and saturated potassium chloride solution and catalyzer, cyclic production once more again.

Embodiment two, in stainless steel interlayer container, add 65 ℃ of hot water, add the solid ammonium sulfate dissolving then, until saturated, add saturated potassium chloride solution again and by 28 ‰ KOH of solution total amount, stir, be cooled to 60 ℃, separate out the vitriolate of tartar after-filtration, the centrifugation solid ammonium sulfate, filtrate and centrifugate are merged, add the bicarbonate of ammonia saturated aqueous solution, keep 60 ℃, separate out for the second time vitriolate of tartar, same spline filter, centrifugation exports to cooling tank with solution, be chilled to 8 ℃, separate out solid ammonium chloride, centrifugation, solution recycles again.

Embodiment three, and ammonium sulfate and saturated solution are added in the stainless steel interlayer reactor, are heated to 75 ℃, add saturated potassium chloride solution again and by 17 ‰ KOH of solution total amount, stir evenly postcooling to 50 ℃, separate out vitriolate of tartar after centrifugation gets K ₂SO ₄, clear liquid adds the saturated carbon aqueous ammonium, keeps 50 ℃, separates out vitriolate of tartar for the second time, and filtration centrifugally goes out K ₂SO ₄, clear liquid is chilled to 15 ℃, separates out ammonium chloride, and centrifugation adds the original raw material cyclic production again in the aqueous solution.

Claims

1. a potassium hydroxide catalysed is produced the method for vitriolate of tartar, with Repone K, ammonium sulfate is main raw material, it is characterized in that, use hot water dissolving's ammonium sulfate of 65-90 ℃ earlier, add Repone K saturated aqueous solution and catalyzer potassium hydroxide by stoichiometric ratio again, the amount that adds catalyzer potassium hydroxide is the 5-30 ‰ of ammonium sulfate and Repone K saturated aqueous solution gross weight, is cooled to 50-60 ℃ after solution is mixed, and separates out vitriolate of tartar, filter then, centrifugation goes out vitriolate of tartar, stays the amount of Repone K according to separating back solution, adds the bicarbonate of ammonia saturated aqueous solution by stoichiometric ratio, mix, keep 50-60 ℃, centrifugation for the second time goes out vitriolate of tartar, and clear liquid is cooled to 5-15 ℃, separate out ammonium chloride crystals, after the centrifugation, mother liquor adds saturated ammonium sulphate, and Repone K and catalyzer be cyclic production once more.