CN1082001A - The preparation vitriolate of tartar in and synthesis method - Google Patents
The preparation vitriolate of tartar in and synthesis method Download PDFInfo
- Publication number
- CN1082001A CN1082001A CN 93104760 CN93104760A CN1082001A CN 1082001 A CN1082001 A CN 1082001A CN 93104760 CN93104760 CN 93104760 CN 93104760 A CN93104760 A CN 93104760A CN 1082001 A CN1082001 A CN 1082001A
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- China
- Prior art keywords
- tartar
- vitriolate
- ammonium sulfate
- synthesis method
- repone
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/02—Preparation of sulfates from alkali metal salts and sulfuric acid or bisulfates; Preparation of bisulfates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of prepare vitriolate of tartar in and synthesis method, it is with sulfuric acid, Repone K, ammonia is raw material, reacts in two steps at a lower temperature, by product is hydrochloric acid and ammonium sulfate.Compare with existing method, it is simple that this method has technology, and cost is low, and reaction safety fast, does not have any loss, and energy consumption is little, is easy to characteristics such as suitability for industrialized production, and the products obtained therefrom quality is good, and the yield height does not contain chlorine, the existence of no free acid.This law is applicable to the production of the agricultural of various scales and industrial sulphuric acid potassium.
Description
The present invention relates to a kind of production method of vitriolate of tartar.
With Repone K is the raw material production vitriolate of tartar, at present, mainly contains three kinds of methods, dry heating method, double decomposition and solvent extrations both at home and abroad.The representative of dry heating method is mannheim (Mannheim) oven process, it is that Repone K and sulfuric acid are mixed the generation sal enixum earlier at a lower temperature, in mannheim furnace, be heated to 500-700 ℃ then, reaction generates vitriolate of tartar, the shortcoming of this method is the desired reaction temperature height, the energy consumption height, seriously corroded, equipment replacement is frequent; Double decomposition is a raw material with Repone K and vitriol, and the shortcoming of this method is that the rate of recovery of potassium is low, and products obtained therefrom purity is low, the chlorinity height, and the processing and the reuse of mother liquor are loaded down with trivial details, and complexity is not easy to industrialized continuous production; Extraction salt acid system and preceding association sulfuric acid process were two kinds after solvent extration was divided into.The shortcoming of this method is that operation steps is more, and the regeneration of the reextraction of solvent or association agent is numerous and diverse, and whole process loss is difficult to more greatly reach a standard on production cost.
The present invention aims to provide a kind of production method of more practical vitriolate of tartar, and at a lower temperature, with sulfuric acid and Repone K, ammonia is raw material, the preparation vitriolate of tartar.
The object of the present invention is achieved like this: Repone K and sulfuric acid reaction at a lower temperature earlier generate sal enixum, and sal enixum neutralizes with ammonia then, generates vitriolate of tartar and ammonium sulfate, and vitriolate of tartar washes with water with ammonium sulfate and separates.
Accompanying drawing 1 and Fig. 2 are whole process flow figure of the present invention, below it are described in detail.
1, the preparation of potassium acid sulfate.
Potassium chloride and sulfuric acid in molar ratio 1: the 0.8-1.4 batching, at room temperature both are mixed first, then heating is warming up to 20-200 ℃ gradually, under stirring state, successive reaction 0.2-6 hour, till overflowing fully to hydrogen chloride gas.
2, the generation of vitriolate of tartar
The sal enixum of above-mentioned generation is added in the reactor, adds an amount of water dissolution, logical ammonia neutralizes, and grasps the feeding amount of ammonia according under meter.The mol ratio of sal enixum and ammonia is 1: 0.7～1.2 for good, and neutralization finishes, and promptly generates vitriolate of tartar, ammonium sulfate or potassium-ammonium sulfate
3, the disassociation of potassium-ammonium sulfate and vitriolate of tartar and ammonium sulfate separates
Because vitriolate of tartar and the very big difference of ammonium sulfate aspect solubleness just can be separated both.With resulting vitriolate of tartar in an amount of water washing (2), ammonium sulfate (or potassium-ammonium sulfate) product can be separated vitriolate of tartar and ammonium sulfate.
Potassium-ammonium sulfate is vitriolate of tartar and ammonium sulfate at dissociation in water
Can obtain agricultural as requested or industrial sulphuric acid potassium product, total consumption of water is 0.5-5 a times of amount of solid, and washing times is 1-5 time.
The present invention adopts neutralisation, react completely, fast, technology is simple, cost is low; Temperature is low, energy consumption is little, little to equipment corrosion, prolong service life of equipment, the transformation efficiency rate of recovery of potassium all reaches more than 99%, and the products obtained therefrom chlorinity is low, purity is high, and quality is good, by product ammonium sulfate can be as fertilizer or compound manure, is applicable to the suitability for industrialized production of vitriolate of tartar of the different size of various scales.
Below by example specific embodiments of the present invention is described:
Example: with 98% sulfuric acid, 272 grams or 93% sulfuric acid, 286.6 grams (rolling over 100% sulfuric acid, 266.6 grams), 96% Repone K, 200 grams (pure Repone K 192.0 grams), 25% ammoniacal liquor, 190 grams (rolling over 100% ammonia, 47.5 grams) with the synthesis method process, separate to such an extent that vitriolate of tartar 235.8 restrains in above-mentioned, hydrochloric acid 266.4 grams, ammonium sulfate 156.9 grams, the rate of recovery of potassium is 99.6%, the rate of recovery of hydrochloric acid is 90%, the vitriolic utilization ratio is 96.7%, and the utilization ratio of ammonia is 92%.
Actual conditions is:
(1) generation of sal enixum
Mole ratio: KCl: H
2SO
4=1: 0.8～1.4
Reaction times: 0.1～3 hour
(2) neutralization
Mole ratio: KHSO
4: NH
3=1: 0.7～1.2
Temperature of reaction: 40 ℃-160 ℃
Reaction times: 0.1～2 hour
(3) separate
Water: Gu=0.5～5: 1
Washing times: 1～5 time
Quality product
Project content chlorinity free acid content
Vitriolate of tartar 94.8%≤0.5% does not have
Hydrochloric acid 32% //
Ammonium sulfate 92.6%≤0.5% does not have
Claims (3)
1, in and synthesis method prepare vitriolate of tartar, it is characterized in that with Repone K, sulfuric acid and ammonia be raw material, reaction is carried out in two steps, the first step, the reaction of sulfuric acid and Repone K generates sal enixum, discharges hydrogenchloride simultaneously, absorbing through water becomes by-product hydrochloric acid; In second step, sal enixum and ammonia carry out neutralization reaction, generate vitriolate of tartar, and by product is an ammonium sulfate, and vitriolate of tartar separates through water washing with ammonium sulfate.
2, in according to claim 1 and synthesis method prepare vitriolate of tartar, it is characterized in that: sulfuric acid and Repone K in molar ratio 1: the 0.8-1.4 batching, be reflected under 20 °-200 ℃ and carry out, sal enixum that generates and ammonia in molar ratio 1: 0.7-1.2 carries out neutralization reaction, temperature is controlled at 40 ℃-160 ℃, and required time is 0.1-2 hour.
3, in according to claim 1 and 2 and synthesis method prepare vitriolate of tartar, it is characterized in that: the separation of potassium-ammonium sulfate, the consumption of washing water be amount of solid 0.5-5 doubly, washing times is 1-5 time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93104760 CN1082001A (en) | 1993-04-23 | 1993-04-23 | The preparation vitriolate of tartar in and synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93104760 CN1082001A (en) | 1993-04-23 | 1993-04-23 | The preparation vitriolate of tartar in and synthesis method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1082001A true CN1082001A (en) | 1994-02-16 |
Family
ID=4985351
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93104760 Pending CN1082001A (en) | 1993-04-23 | 1993-04-23 | The preparation vitriolate of tartar in and synthesis method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1082001A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042823C (en) * | 1994-05-17 | 1999-04-07 | 化学工业部长沙化学矿山设计研究院 | Method for preparation of lemery salt |
| CN1125776C (en) * | 1999-01-27 | 2003-10-29 | 青岛科技大学 | Metathesis process for producing potassium sulfate in ammonia/water medium |
| CN1789129B (en) * | 2005-12-12 | 2010-10-06 | 中国科学院青海盐湖研究所 | Method for extracting potassium sulphate by magnesium sulfate sub-type potassium-containing salt lake brine water |
| CN105502439A (en) * | 2016-01-22 | 2016-04-20 | 金正大生态工程集团股份有限公司 | Method for producing potassium sulfate by-product ammonium potash chloride through low-temperature conversion |
| CN107226457A (en) * | 2017-08-01 | 2017-10-03 | 武汉江汉化工设计有限公司 | A kind of wire rope factory abraum salt acid treatment device and the method for processing application |
-
1993
- 1993-04-23 CN CN 93104760 patent/CN1082001A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042823C (en) * | 1994-05-17 | 1999-04-07 | 化学工业部长沙化学矿山设计研究院 | Method for preparation of lemery salt |
| CN1125776C (en) * | 1999-01-27 | 2003-10-29 | 青岛科技大学 | Metathesis process for producing potassium sulfate in ammonia/water medium |
| CN1789129B (en) * | 2005-12-12 | 2010-10-06 | 中国科学院青海盐湖研究所 | Method for extracting potassium sulphate by magnesium sulfate sub-type potassium-containing salt lake brine water |
| CN105502439A (en) * | 2016-01-22 | 2016-04-20 | 金正大生态工程集团股份有限公司 | Method for producing potassium sulfate by-product ammonium potash chloride through low-temperature conversion |
| CN107226457A (en) * | 2017-08-01 | 2017-10-03 | 武汉江汉化工设计有限公司 | A kind of wire rope factory abraum salt acid treatment device and the method for processing application |
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| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |