CN1104178A

CN1104178A - Method for production of Lemery salt

Info

Publication number: CN1104178A
Application number: CN 94117425
Authority: CN
Inventors: 何永汉
Original assignee: He Binsheng; He Liujing
Current assignee: He Binsheng; He Liujing
Priority date: 1994-11-01
Filing date: 1994-11-01
Publication date: 1995-06-28
Anticipated expiration: 2014-11-01
Also published as: CN1041401C

Abstract

The invention is a method of producing potassium sulfate with sulphuric acid, ammonium bicarbonate, potassium chloride as the main raw materials. The method is characterized in that the potassium sulfate is produced in one step when the PH is 6-7, and then the potassium sulfate and ammonium chloride are precipitated in the different temperature. The whole process is simple; the energy consumption and pollution is light; the requirement for the equipment is not high, and the production cost is low.

Description

Method for production of Lemery salt

The present invention relates to a kind of is the method for main material production vitriolate of tartar with Repone K.

Vitriolate of tartar is important industrial raw material, and agricultural goes up important inorganic chemical fertilizer commonly used especially, and the many cash crop that can not use Repone K such as sugarcane, tobacco, tealeaves, watermelon, jute, citrus must not contain Cl with vitriolate of tartar or potassium primary phosphate etc. ^-Potash fertilizer.Present being seen vitriolate of tartar production method has following several: 1. Repone K and sulfuric acid react in the strong acid pyrosol, generate vitriolate of tartar and hydrochloric acid; Sodium sulfate and Repone K be raw material through twice transformation, vitriolate of tartar is produced in single vaporization; 3. be that vitriolate of tartar and side product sodium chloride are produced in raw material metathesis under mesophilic condition with ammonium sulfate and Repone K.The weak point that above-mentioned several method exists is: the 1st kind of method is that facility investment is big, needs the acid-resistant and anti-high-temperature material, and free acid is arranged, and corrosion and pollution are more serious; The 2nd kind of method is to pass through twice transformation and evaporation, complex procedures, and equipment is many, difficult operation; The 3rd kind of method is that replacement(metathesis)reaction is slow, and input-output ratio is little, and the ammonium sulfate cost is higher, and the whole production cost is also improved thereupon.

It is low to the purpose of this invention is to provide a kind of energy consumption and cost, little to equipment corrosion, and speed of response is fast, no free acid, the production method of the vitriolate of tartar that yield is high.

The method that the present invention realizes is that the pH value to solution obtained vitriolate of tartar and ammonium chloride near adding the Repone K reaction under the neutral condition after sulfuric acid mixed with bicarbonate of ammonia, isolates vitriolate of tartar and ammonium chloride then under different temperature.

Chemical reaction of the present invention is as follows:

The side reaction that exists may for:

Below be specific embodiment:

1. the sulfuric acid of 30-50% being added in the dissolving tank that is placed with solid ammonium bicarbonate (also can utilize existing carbon ammonium factory carbodiimide solution to add the vitriol oil), when the pH of solution reaches 6-7, add the Repone K saturated aqueous solution again, and the temperature of solution risen to 50-65 ℃, stir, insulation was left standstill more than half an hour, can separate out K ₂SO ₄Crystal, as begin reaction and separate out slowly, can add small amount of solid K earlier ₂SO ₄Help crystallization.

2. with the above-mentioned K that obtains ₂SO ₄And the solution filtration, and be put into immediately in the whizzer K ₂SO ₄Separate.

3. isolating solution is chilled to normal temperature (20-30 ℃), can separates out NH ₄Cl crystallization and a spot of (NH ₄) ₂SO ₄,, obtain NH through centrifugation ₄Cl and mother liquor.

4. the mother liquor after separating flows back to dissolving tank, adds bicarbonate of ammonia and sulfuric acid, repeats above-mentioned processing step, can continuously produce K ₂SO ₄And NH ₄Cl.

Advantage of the present invention: 1. adopted the bicarbonate of ammonia that the source is easy, price is low, made production cost reduce about 1/4 than existing several method; 2. equipment is simple, can adopt the popular response device, the also lined easy reactor of used water mud sump, and investment only is 1/4 of traditional vitriolate of tartar equipment; 3. carry out under the condition that total overall reaction is neutral at PH substantially and temperature is not high, alleviated the corrosion of equipment and saved the energy than prior art; 4. the mother liquor after the Reaction Separation can be recycled, no free acid, and no waste liquid waste gas produces, and environment is not impacted.

Below be embodiments of the invention:

Embodiment one, adds 800 kilograms in the sulfuric acid of 600 kilograms of bicarbonate of ammonia and 40% in dissolving tank, when the pH value for the treatment of solution is 6-7, in advance 550 kilograms of Repone K are added water and obtain saturated solution, saturated potassium chloride solution is added in the dissolving tank mixes, about reheat to 55 ℃, can separate out K ₂SO ₄, then with the K that contains of lower floor ₂SO ₄Solid be put into and isolate solid in the whizzer, solution continues to be chilled to about 25 ℃, (pH is about between the 6-7) NH ₄Cl separates out, again with solids constituent from, mother liquor is drawn back in the dissolving tank again, continue to add sulfuric acid and bicarbonate of ammonia, cyclical operation again.

Embodiment two, industrial sulphuric acid with 90% is added in the liquid storage vessel after the carbonization of carbonization workshop section of carbon ammonium factory, liquid-solid ratio is 60-65% after the carbonization, adding the vitriolic amount is metered into by chemical equation of the present invention, notice that the pH value transfers to 6-7, be warming up to 60 ℃, add the KCl saturated aqueous solution again, keep temperature, separate out K ₂SO ₄After crystallization be extracted into whizzer separate, be chilled to again about 30 ℃, separate out NH ₄Cl, centrifugation adds ammonia with this solution and continues to absorb CO ₂

The product that the present invention produces is measured potassium (K through provincial product quality supervision and testing institute by the method for the specialized standard ZBG21006-89 of the People's Republic of China (PRC) " potassium sulfate for agricultural use " ₂O) content is 47.0%, and muriate (Cl) is 2.4, byproduct NH ₄Cl content reaches 16.9%, reaches the acceptable end product index.

Claims

1, a kind of method of producing vitriolate of tartar, its main raw material comprises sulfuric acid, Repone K, it is characterized in that: the saturated aqueous solution that adds Repone K when sulfuric acid is earlier reacted pH6-7 to solution with bicarbonate of ammonia, the temperature of solution is heated to 50-65 ℃, after the vitriolate of tartar Crystallization Separation of separating out, reduce to 20-30 ℃ again, the ammonium chloride of fractional crystallization, mother liquor recycles again.

2, the method for production vitriolate of tartar according to claim 1 is characterized in that bicarbonate of ammonia is solid or synthetic ammonia stone carbodiimide solution.

3, the method for production vitriolate of tartar according to claim 1, it is characterized in that adding the Repone K saturated aqueous solution after, can add solid sulphuric acid potassium crystallization in motion.