CN1076317C

CN1076317C - Process for producing potassium sulfate

Info

Publication number: CN1076317C
Application number: CN98112323A
Authority: CN
Inventors: 彭赛军
Original assignee: Individual
Current assignee: Individual
Priority date: 1998-01-21
Filing date: 1998-01-21
Publication date: 2001-12-19
Anticipated expiration: 2018-01-21
Also published as: CN1223964A

Abstract

The present invention provides a production technology for potassium sulfate, which belongs to the technical field of inorganic chemical industry. The production technology for potassium sulfate mixes sodium sulfate carriers of sodium sulfate, or mirabilite, or sodium sulfate solution, etc., potassium chloride, salt preparing mother solution, water, etc. which are taken as raw materials according to a definite distribution ratio to carry out double decomposition reaction, and potassium preparing mother solution and rough potassium sulfate can be obtained by separation; then, the potassium preparing mother solution is evaporated, and the rough potassium sulfate and the potassium sulfate solution are mixed according to a definite distribution ratio to carry out thermal melting washing, separation by cooling and refined granulating, and the potassium sulfate finished products and sodium chloride byproducts can be obtained by separation. The present invention has the characteristics of high quality of main products and byproducts, high value, high utilization rate of raw materials, low cost, low energy consumption, no discharge of three wastes, etc.

Description

Process for producing potassium sulfate

The present invention be a kind of be the process for producing potassium sulfate of main raw material with sodium sulfate carrier and Repone K, belong to technical field of inorganic chemical industry.

The known method of producing vitriolate of tartar and byproduct sodium-chlor with sodium sulfate and Repone K conversion, there are two sections to transform mother liquid evaporation method and two sections conversion mother liquor cold methods, but wherein two sections transform in the mother liquid evaporation method glaserite mother liquid evaporation and separate out sodium sulfate and sodium-chlor mixing salt, influence the rate of recovery of product cost and quality and sodium sulfate, and wherein two sections freezing rules of conversion mother liquor exist technical process length, investment, energy consumption and the high problem of product cost, therefore, in fact above-mentioned two methods are difficult to carry out.

The present invention is directed to the problems referred to above, change the operational path that sodium sulfate and Repone K are produced vitriolate of tartar, simplify the reaction hop count, propose one and can cut down the consumption of energy and cost the process for producing potassium sulfate that improves the quality of products.

Solution of the present invention is to propose one with the sodium sulfate carrier, for example sodium sulfate (Na ₂SO ₄), saltcake (Na ₂SO ₄-10H ₂O) or metabisulfite solution (Na ₂SO ₄Solution) be the process for producing potassium sulfate of main raw material with Repone K, this technology is taken sodium sulfate or saltcake or metabisulfite solution and (is pressed Na ₂SO ₄The composition meter), Repone K, salt-making mother liquor and water are successively by the mixed replacement(metathesis)reaction of carrying out of 1: 1～1.05: 5～10: 0.1～2.5 composition by weight, 0.5～4 hour reaction times, 15～50 ℃ of invert points, carry out solid-liquid separation then and must make potassium mother liquor and rough vitriolate of tartar, high temperature evaporation system potassium mother liquor wherein makes it to carry out solid-liquid separation behind the condensing crystal and gets salt-making mother liquor and byproduct sodium-chlor, this salt-making mother liquor participates in the above-mentioned replacement(metathesis)reaction of circulation down, and above-mentioned rough vitriolate of tartar adds potassium sulfate solution and carries out thermosol washing and cold analysis granulation by 1: 1～12 components by weight percent are mixed, thermosol washing time 0.1-4 hour, 25-100 ℃ of thermosol wash temperature, 15-75 ℃ of cold analysis temperature, carry out solid-liquid separation get product vitriolate of tartar and potassium sulfate mother liquid then, this potassium sulfate mother liquid participates in the above-mentioned thermosol washing of circulation down cold analysis granulating working procedure.In the above-mentioned technological process, the theoretical rate of recovery of sodium sulfate and Repone K is 100%, has significantly than the rate of recovery of known technology 50-83% and improves, and the first grade standard that quality of potassium sulfate reaches country's song cloth (contains potassium oxide K ₂O＞45%, chlorine root Cl＜2.5%), granularity 0.1-4mm, byproduct sodium-chlor reach country's song cloth edible salt first grade standard (sodium chloride-containing NaCl＞98.5%, whiteness＞70), granularity 0.15-0.35mm.One ton of vitriolate of tartar of every product (contains potassium oxide K ₂O45% counts) and 0.56 ton of sodium-chlor (sodium chloride-containing NaCl98.5% meter) consumption sodium sulfate (contains sodium sulfate Na ₂SO ₄98%) 0.72 ton, 0.83 ton in Repone K (containing Repone K KCl90% meter), and technological process does not have waste liquid and discharges, (price of vitriolate of tartar is 2 times of Repone K price to have major-minor value of the product height, the price of sodium-chlor is 1-20 a times of saltcake), raw material availability and product and byproduct quality height, energy consumption is low, characteristics such as the low and three-waste free discharge of production cost.

Embodiment 1: get 0.833 ton of anhydrous sodium sulphate and (contain Na ₂SO ₄98%), 0.945 ton of Repone K (containing the Kcl90% meter), 5.667 tons of salt-making mother liquors, 2.041 tons of water are gone into jar and are mixed, and stir 3 hours under 20 ℃ of temperature, get 1.0 tons of rough vitriolate of tartar and 8.485 tons of system potassium mother liquors by solid-liquid separation after this replacement(metathesis)reaction.

8.485 tons of system potassium mother liquors are flashed to salt-making mother liquor under 100 ℃ of temperature, get 0.667 ton of sodium-chlor and 5.667 tons of salt-making mother liquors after the solid-liquid separation.5.667 tons of salt-making mother liquors are cooled to 20 ℃ participate in next above-mentioned replacement(metathesis)reaction that circulates.

1.0 tons of potassium sulfate solutions of above-mentioned 1.0 tons of rough vitriolate of tartar addings are gone into jar to be mixed, stir under 100 ℃ of temperature and carried out thermosol detergent manufacturing grain in 1 hour, be cooled to 25 ℃, get 1.0 tons of vitriolate of tartar and 1.0 tons of potassium sulfate mother liquids by solid-liquid separation again, this potassium sulfate mother liquid participates in next above-mentioned thermosol detergent that circulates and makes the grain operation.

Embodiment 2: get 2.04 tons of mirabilite hydrates and (contain Na ₂SO ₄40%), 0.945 ton of Repone K (containing the Kcl90% meter), it is jar mixed that 5.66 tons of salt-making mother liquors, 0.919 ton of water are gone into, and stirred 3 hours under 20 ℃ of temperature, gets 1.0 tons of rough vitriolate of tartar and 8.485 tons of system potassium mother liquors by solid-liquid separation after this replacement(metathesis)reaction.

8.485 tons of system potassium mother liquors are flashed to salt-making mother liquor under 100 ℃ of temperature, get 0.667 ton of sodium-chlor and 5.667 tons of salt-making mother liquors after the solid-liquid separation.5.667 tons of salt-making mother liquors are cooled to 25 ℃ participate in next above-mentioned replacement(metathesis)reaction that circulates.

11.0 tons of potassium sulfate solutions of above-mentioned 1.0 tons of rough vitriolate of tartar addings are gone into jar to be mixed, stir under 100 ℃ of temperature and carried out thermosol detergent manufacturing grain in 2 hours, be cooled to 20 ℃, get 1.0 tons of product vitriolate of tartar and 11.0 tons of potassium sulfate mother liquids by solid-liquid separation again, this potassium sulfate mother liquid participates in next above-mentioned thermosol detergent that circulates and makes the grain operation.

Embodiment 3: get 2.843 tons of metabisulfite solutions and (contain Na ₂SO ₄Be 345g/L, proportion 1.2), 0.3 ton in 0.945 ton of Repone K (KCl.90% meter), 5.667 tons of salt-making mother liquors and water goes into jar mixed, stirred 2 hours under 25 ℃ of temperature, after this replacement(metathesis)reaction, get 1.0 tons of rough vitriolate of tartar and 8.485 tons of system potassium mother liquors by solid-liquid separation.

8.485 tons of system potassium mother liquors are flashed to salt-making mother liquor under 105 ℃ of temperature, get 0.667 ton of sodium-chlor and 5.667 tons of salt-making mother liquors after the solid-liquid separation.5.667 tons of salt-making mother liquors are cooled to 25 ℃ participate in next above-mentioned replacement(metathesis)reaction that circulates.

1.0 tons of potassium sulfate solutions of above-mentioned 1.0 tons of rough vitriolate of tartar addings are gone into jar to be mixed, stir under 100 ℃ of temperature and carried out thermosol detergent manufacturing grain in 0.5 hour, be cooled to 25 ℃, get 1 ton of vitriolate of tartar and 1 ton of potassium sulfate mother liquid by solid-liquid separation again, this potassium sulfate solution participates in next above-mentioned thermosol detergent that circulates and makes the grain operation.

Claims

1, a kind of with sodium sulfate and Repone K process for producing potassium sulfate as raw material, it is characterized in that it takes sodium sulfate, Repone K, salt-making mother liquor and water are successively by the mixed replacement(metathesis)reaction of carrying out of 1: 1～1.05: 5～10: 0.1～2.5 composition by weight, 0.5～4 hour reaction times, 15～50 ℃ of invert points, carry out solid-liquid separation then and must make potassium mother liquor and rough vitriolate of tartar, high temperature evaporation system potassium mother liquor wherein makes it to carry out solid-liquid separation behind the condensing crystal and gets salt-making mother liquor and byproduct sodium-chlor, this salt-making mother liquor participates in the above-mentioned replacement(metathesis)reaction of circulation down, and above-mentioned rough vitriolate of tartar adds potassium sulfate solution and carries out thermosol washing and cold analysis granulation by 1: 1～12 components by weight percent are mixed, thermosol washing time 0.1-4 hour, 25-100 ℃ of thermosol wash temperature, 15-75 ℃ of cold analysis temperature, carry out solid-liquid separation get product vitriolate of tartar and potassium sulfate mother liquid then, this potassium sulfate mother liquid participates in the above-mentioned thermosol washing of circulation down cold analysis granulating working procedure.

2, process for producing potassium sulfate according to claim 1 is characterized in that the described sodium sulfate of thing also can be as an alternative: saltcake or metabisulfite solution.