CN1047367C - Process for producing potassium sulfate - Google Patents
Process for producing potassium sulfate Download PDFInfo
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- CN1047367C CN1047367C CN95117034A CN95117034A CN1047367C CN 1047367 C CN1047367 C CN 1047367C CN 95117034 A CN95117034 A CN 95117034A CN 95117034 A CN95117034 A CN 95117034A CN 1047367 C CN1047367 C CN 1047367C
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- potassium
- tartar
- vitriolate
- sulfuric acid
- solid
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Abstract
The present invention relates to a method by utilizing water to decompose/ leach solid potassium bisulfate to prepare solid potassium sulfate products and water solution of sulfuric acid. The water solution of sulfuric acid can be used for producing solid potassium bisulfate after being evaporated and concentrated. The prepared potassium sulfate product has the chlorine content smaller than 0.5%, and the potassium oxide content more than 50%.
Description
The invention belongs to chemical technology field, relate to a kind of method of producing vitriolate of tartar.
Vitriolate of tartar is widely used in the production of cash crop such as tobacco, fruit as chlorideless potassic fertilizer.Potassium is one of N, P, K three big nutritive elements of farm crop, and sulphur also is middle amount nutritive element, thereby vitriolate of tartar is used to produce compound fertilizer special in a large number as K, S double base fertilizer, supplies with cash crop and uses.
At present, the method for producing vitriolate of tartar mainly contains: with Repone K and sulfuric acid is the Mannbeim method of raw material, and CN1059132A forms the method for putting, the organic amine solvent extration of CN1089575A etc.; With sal epsom, ammonium sulfate or sodium sulfate and Repone K is the double decomposition of raw material; Alunite reduction heat solution.
The present invention is the method that obtains solid sulphuric acid potassium with water decomposition solid sulphuric acid hydrogen potassium.The solid sulfur potassium hydrogen phthalate is that raw material makes with sulfuric acid and Repone K.Its method can be with 50～98% vitriolization Repone K, and at 70～160 ℃, with 1～20: 1 mol ratio is reacted, and generates sal enixum and hydrogenchloride, and the hydrogenchloride water absorbs and makes hydrochloric acid or make ammonium chloride with the ammonia neutralization.The aqueous sulfuric acid of reacted sal enixum is isolated the solid sulfur potassium hydrogen phthalate through crystallisation by cooling.The preparation method of relevant sal enixum all has narration at DE4111718A among CN1059132A and the CN1097178A.
The objective of the invention is: be that raw material makes on the basis of solid sulfur potassium hydrogen phthalate with Repone K and sulfuric acid, the vitriolate of tartar that puts into production with try one's best few machining medium (process water) and equipment reduces production costs, and enhances the competitiveness.
The object of the present invention is achieved like this, under 0～50 ℃ temperature, obtains the product and the aqueous sulfuric acid of solid sulphuric acid potassium with an amount of water decomposition sal enixum.Aqueous sulfuric acid is through the raw material of evaporation concentration as production solid sulfur potassium hydrogen phthalate.The water that evaporates from aqueous sulfuric acid can be used for decomposing the solid sulfur potassium hydrogen phthalate after condensation, thereby forms circulation.
Method of the present invention is that machining medium decomposition solid sulfur potassium hydrogen phthalate obtains solid sulphuric acid potassium product with water.From the angle of unit operation, this course of processing is the process of a liquid-solid extraction or leaching (going out), and promptly water is transferred to the sulfuric acid in the solid sulfur potassium hydrogen phthalate the liquid phase (water) from solid phase, and remaining solid is vitriolate of tartar.
Method of the present invention is compared as the method for machining medium with organic amine, has the course of processing simple, does not have organic amine to pollute potassium product and organic amine consumption, thereby the quality product height, and production cost is low, and is pollution-free.
Method of the present invention at 0～50 ℃, is that substep (level) carries out with the process of water decomposition/extraction (leaching) solid sulfur potassium hydrogen phthalate.Sal enixum is seen as sulfuric acid and the formed double salt of vitriolate of tartar, during with this double salt of water decomposition, can be divided into two-step approach and three-step approach and produce vitriolate of tartar, also can use multistep (more than three steps) method and continuous countercurrent technique to produce vitriolate of tartar.Isolated solid is the mixing salt of vitriolate of tartar and sal enixum in the middle of in two-step approach, and its vitriolate of tartar content is 70～84%.In three-step approach, two solidss are isolated in the centre, the isolated solids of the first step is the vitriolate of tartar of sulfur acid potassium 85～80% and the mixing salt of sal enixum, and second step, isolated solid was the vitriolate of tartar of sulfur acid potassium 75～85% and the mixing salt of sal enixum.Isolate the pairing mother liquor of mixing salt and vitriolate of tartar and can return processing mixing salt or sal enixum.Decomposing the formed aqueous sulfuric acid of sal enixum can be directly or through the raw material of evaporation concentration as manufacturing solid sulfur potassium hydrogen phthalate, thereby from sulfuric acid and Repone K being the consideration on the whole of the raw material whole technological process of producing vitriolate of tartar, aqueous sulfuric acid has formed closed cycle, process water uses through evaporation, condensation cycle as machining medium, when producing potassium product, pay and produce hydrogenchloride or hydrochloric acid, also available ammonia neutralization makes ammonium chloride.
Method of the present invention is under 0～50 ℃ of temperature, produces vitriolate of tartar with water decomposition solid sulphuric acid hydrogen potassium.The water yield that decomposition/leaching solid sulfur potassium hydrogen phthalate is used, by substep situation (two steps of processing, three step or multisteps) and the logistics direction of solid materials (sal enixum and mixing salt) and liquid material (water and respectively go on foot corresponding mother liquor) (contrary, also, cross-flow or three kinds of flow directions combine) different, the total water amount of every output 1 mol sulfuric acid potassium solid phase prod is 8～50 moles; Just every production 1 mol sulfuric acid potassium solid phase prod need evaporate 8～50 moles water.The reaction times of per step decomposition reaction is 1～55 minute.
The present invention is further illustrated below by embodiment.
Embodiment one:
The first step: take by weighing 450 gram sal enixum solids and drop in the glass beaker of 500ml down in room temperature (30 ℃), add 260ml water and second and go on foot mother liquor 240 grams of isolating vitriolate of tartar, with the glass stick stirring reaction after 20 minutes, pour the method for using vacuum filtration in the sand core funnel into, get mixing salt 180 grams of sulfur acid potassium 84%; Second step: 180 gram mixing salts are poured in the beaker of 500ml, under room temperature (30 ℃), added 160ml water, with the glass stick stirring reaction after 10 minutes, suction filtration in sand core funnel gets vitriolate of tartar solid 96 grams, and mother liquor returns the first step and initiate water decomposes sal enixum together.
Embodiment two:
The first step: take by weighing 220 gram sal enixum solids in the 500ml glass beaker, under 20 ℃, add 75 gram water and added for second step and the isolated mother liquor of the 3rd step institute 176 restrains totally, with glass stick stirring reaction 40 minutes, the mixing salt I 116 that gets sulfur acid potassium 74% with glass sand core funnel vacuum filtration restrains, and isolated mother liquor is used to produce sal enixum through evaporation concentration.Second step: under 20 ℃, the mixing salt I of the first step gained is placed on adds 70 gram water in the 500ml beaker, stirring reaction is after 15 minutes, gets mixing salt II 73 grams of sulfur acid potassium 82.5% with the sand core funnel vacuum filtration, and mother liquor returns the first step processing sal enixum.The 3rd step; Under 20 ℃, in the 250ml beaker, add entry 40 grams by obtained 73 gram mixing salt II of second step, stirring reaction is after 5 minutes, with sand core funnel filter vitriolate of tartar solid phase prod 50 grams, mother liquor returns the first step and handles sal enixum.
Embodiment three:
The mother liquor (M1) that adds 57 gram 98% sulfuric acid and got by separate sulfur potassium hydrogen phthalate solid in the three neck glass reaction bottles of 1000ml is through sulphuric acid soln 800 grams of evaporation concentration to 70%, add 86 gram Repone K, be heated to 100～120 ℃ of reactions, with hydrogenchloride drive out of and water absorb hydrochloric acid.Reaction residual liquor mixes with the decomposition resulting mother liquor of sal enixum (M2) and is cooled to 30 ℃, gets solid sulfur potassium hydrogen phthalate crystallization 262 grams with the sand core funnel vacuum filtration, and mother liquor (M1) is produced sal enixum with the Repone K reaction together through evaporation concentration and sulfuric acid.
The solid sulfur potassium hydrogen phthalate can make potassium product by the method processing of three steps adverse current decomposition/leaching.One step of the mat woven of fine bamboo strips: sal enixum 262 grams are under 10 ℃, in the 800ml beaker, decomposed resultant mother liquor (M3) 440 gram stirring reactions 45 minutes with second step, with sand core funnel filter mixing salt I 320 gram of sulfur acid potassium 66%, mother liquor (M2) is used to produce sal enixum as stated above.Second step: 320 gram mixing salt I are decomposed resulting mother liquor (M4) 350 grams with the 3rd step in the 500ml beaker, stirring reaction 15 minutes, with sand core funnel filter mixing salt II 230 gram of sulfur acid potassium 77%, mother liquor (M3) returns the first step and is used to decompose sal enixum.The 3rd step: 230 gram mixing salt II and 225 gram water, 40 ℃ of following stirring reactions after 10 minutes in the 500ml beaker, with sand core funnel filter vitriolate of tartar solid 104 grams, mother liquor (M4) returned for second step and is used to decompose the mixing salt I.
The potassium product quality
Repone K (K
2O) content: 50,20%
Chlorine (Cl) content: 0.16%
Moisture content: 0.5%
Claims (3)
1. method of producing vitriolate of tartar, it is characterized in that: obtain solid sulphuric acid potassium and aqueous sulfuric acid with water decomposition/leaching solid sulfur potassium hydrogen phthalate, isolated vitriolate of tartar is product; The water yield that the solid sulfur potassium hydrogen phthalate is decomposed/leaches in required being used to of every output 1 mol sulfuric acid potassium is 8～50 moles; Aqueous sulfuric acid can be used for production solid sulfur potassium hydrogen phthalate through evaporation concentration, forms circulation.
2. method according to claim 1 is characterized in that: the temperature with water decomposition solid sulphuric acid hydrogen potassium is 0～50 ℃.
3. method according to claim 1 is characterized in that: produce vitriolate of tartar with water decomposition/leaching solid sulfur potassium hydrogen phthalate and can adopt two steps, three steps, multistep or continuous countercurrent technique to carry out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95117034A CN1047367C (en) | 1995-10-19 | 1995-10-19 | Process for producing potassium sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95117034A CN1047367C (en) | 1995-10-19 | 1995-10-19 | Process for producing potassium sulfate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1130596A CN1130596A (en) | 1996-09-11 |
| CN1047367C true CN1047367C (en) | 1999-12-15 |
Family
ID=5081105
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95117034A Expired - Fee Related CN1047367C (en) | 1995-10-19 | 1995-10-19 | Process for producing potassium sulfate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1047367C (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1089575A (en) * | 1993-01-08 | 1994-07-20 | 中国科学院青海盐湖研究所 | Benzene is followed the example of and is produced potassium sulfate process |
-
1995
- 1995-10-19 CN CN95117034A patent/CN1047367C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1089575A (en) * | 1993-01-08 | 1994-07-20 | 中国科学院青海盐湖研究所 | Benzene is followed the example of and is produced potassium sulfate process |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1130596A (en) | 1996-09-11 |
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