CN102476790A - Method for preparing hydrochloric acid and potassium carbonate by adopting KCl as raw material with molten hydrolysis method - Google Patents
Method for preparing hydrochloric acid and potassium carbonate by adopting KCl as raw material with molten hydrolysis method Download PDFInfo
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- CN102476790A CN102476790A CN2010105656292A CN201010565629A CN102476790A CN 102476790 A CN102476790 A CN 102476790A CN 2010105656292 A CN2010105656292 A CN 2010105656292A CN 201010565629 A CN201010565629 A CN 201010565629A CN 102476790 A CN102476790 A CN 102476790A
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- hydrochloric acid
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- salt
- wormwood
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Abstract
The invention relates to a new method for directly preparing hydrochloric acid and potassium carbonate by a potassium chloride molten hydrolysis method. The method is characterized in that: the special characteristic of KB5O8 in the molten state is adopted; potassium chloride and KB5O8 are subjected to melting and mixing, and superheated steam is introduced, such that hydrogen ions in the system and chloride ion in the system are combined to generate hydrogen chloride gas; the hydrogen chloride gas and the remaining steam after the reaction are mixed and condensed to generate the hydrochloric acid solution; the generated alkali metal borate during the reaction process is subjected to water quenching and carbonation to regenerate the KB5O8.4H2O, wherein the B2O3/K2O ratio of the alkali metal borate becomes small; the KB5O8.4H2O is dried to recycle; the KHCO3 solution is obtained when the carbonation treatment is performed to regenerate the KB5O8.4H2O, and is subjected to a further treatment to obtain the K2CO3.
Description
Technical field
The invention belongs to the bittern chemical industry, relate to a kind of industrial potassium chloride that utilizes and be raw material, as middle circulatory mediator, high-temperature fusion attitude hydrolytic reactions prepares hydrochloric acid earlier with potassium pentaborate, and again through carbonation, the back prepares the method for salt of wormwood product.
Background technology
Salt of wormwood is one of important basic inorganic chemical industry, medicine, light industry raw material, is mainly used in opticglass, welding electrode, valve, kinescope, bulb, printing and dyeing, dyestuff, printing ink, the medicine of taking pictures, bubble flower alkali, polyester, explosive, plating, process hides, pottery, building materials, crystal, soap and production of medicine; Also can be used as and contain potassic fertilizer, adsorbent, powder extinguishing agent, rubber antioxidant, and the carbonic acid gas that is used for removing the chemical fertilizer synthetic gas.Along with continually developing of new and high technology, salt of wormwood is at washing auxiliary detergent, monosodium glutamate, and the application in fields such as food also enlarges day by day.At present, salt of wormwood is mainly used in potassic glass, SOFT SOAP, and other inorganic chemicals manufacturings, is used for removing the hydrogen sulfide and the carbonic acid gas of industrial gasses, also is used for aspects such as welding electrode, printing ink manufacturing, printing and dyeing industry.
Salt of wormwood production has plant ash method, leblanc process, electrolytic process, ion exchange method etc.Commonly used is electrolytic process and ion exchange method.The plant ash method is the most ancient method, promptly from the plant ash that various plant shells (like cotton seed hulls, tea shell, seeds of a tung oil tree shell, Semen Helianthi shell) burn till, extracts.Contain soluble salts such as salt of wormwood, vitriolate of tartar, Repone K in the plant ash, can separate with deposition, filtering method.This method is low, uneconomical owing to quality product, and receives the raw material sources restriction and seldom employing.Leblanc process is that vitriolate of tartar is mixed with coal dust, lime, reducing roasting, grey black (carbonated potassium, sulfurated lime etc. burn till thing), through leaching, filtration, evaporation, carbonization, saleratus, again through filter, calcine product; This method is owing to reasons such as technical process length are replaced by additive method.
Electrolytic process is the potassium hydroxide solution that obtains after the Repone K electrolysis, in carbonating tower with the carbonic acid gas carbonization; Evaporate, filter excessively saleratus through multiple-effect evaporator; Make product through calcining again.This method is because of raw material is easy to get, the potassium utilization ratio high, the no three wastes produce and are used widely, but power consumption is bigger.
Ion exchange method is with Zeo-karb and Repone K exchange.Become the saleratus dilute solution with the bicarbonate of ammonia wash-out again, through multiple-effect evaporation, carbonization, crystallization, separation, calcine product; This method good product quality, technical process weak point, but only be applicable to small-scale production.
The inventive method is to utilize the reaction of Repone K and borate high-temperature fusion attitude, and the cl ions in the Repone K is made product with the form of hydrochloric acid, contains the potassium fused salt and then carries out carbonating, produces salt of wormwood.The chemical reaction process of present method is not seen bibliographical information, and operational path is short simultaneously, has formed the method that brand-new melt hydrolysis method prepares hydrochloric acid and salt of wormwood.
Summary of the invention
A kind of Repone K melt hydrolysis method is directly produced hydrochloric acid and salt of wormwood novel method, and described melt hydrolysis is under alkali metal chloride is in molten state, feeds superheated vapour, and the hydrolysis reaction under the molten state is called " melt hydrolysis ".Its cardinal principle is following:
The total reaction balanced type:
Reaction formula (1) expression KCl solid and KB
5O
8Crystal mixing post-heating to 800～1200 ℃ of congruent meltings is with superheated vapour reaction, KB more than 800 ℃
5O
8Have acidity after the fusion, can sour environment be provided for the decomposition of KCl; Cl in the melt
-Be hydrolyzed into gas HCl, with reaction back remainder water steam, and and melt extraction, become hydrochloric acid soln after the condensation; Melt KBO
2(reality is B
2O
3/ K
2The ratio of O is a borate less than 2 serial K, i.e. K
2B
4O
7To K
4B
2O
5Between many potassium borates, be mainly K
2B
4O
7) direct shrend pulping liquid.Reaction formula (2) is represented these slurries and CO
2Gas reaction, carbonation reaction temperature are 30～40 ℃, pressure 0.1～0.3Mpa, and Tc is 10～15 ℃, generates KB
5O
84H
2O crystallization and KHCO
3Near saturated solution is through filtering KB
5O
84H
2The O crystal returns, and drying is mixed congruent melting hydrolysis again with new KCl solid after taking off crystal water.Filter gained KHCO
3Near saturated solution is through the refining Cl that removes
-,
Ion, thermolysis get the clean K of pure d
2CO
3Product.This method is mainly utilized KB
5O
8The characteristic that solubleness is little realizes reprocessing cycle easily, and carbonation CO
2Dividing potential drop 1Kg/cm
2Can meet the demands.
Described superheated vapour is that temperature reaches more than 200 ℃, but pressure is non-pressurized superheated vapour.
Compare with existing relieving haperacidity system alkali method, the present invention has following advantage:
(1) there is not Ca
2+Participate in, must CaCO
3Make raw material, broken away from the limestone kiln of high energy consumption.
(2) technical process is brief, realizes the transforming agent reprocessing cycle through crystallization, processing ease, and facility investment is little.
(3) high-temperature molten salt reaction contains HCl gas, is easy to recycle with the heat energy of melt, and total energy consumption is low.
(4) industrial scale is changeable, is easy to make up cleaner production and recycling economy system, produce in situ, in-field use, has avoided hydrochloric acid in the difficulty of storing with transit link, but even high temperature HCl diluents direct chemical absorb.
(5) the HCl use is wide, can be easy to change into Cl
2Gas under certain condition will be than electrolysis legal system Cl
2Gas is superior, does not have H
2Association, energy consumption is low, invests little.
Description of drawings
Accompanying drawing 1 is to be circulatory mediator with the potassium pentaborate, and Repone K is the technical process of feedstock production hydrochloric acid and salt of wormwood;
Embodiment
Get a certain amount of Repone K and mix with potassium pentaborate, be made into the fusion of solid powder post-heating, place reactor drum, feed superheated vapour and react, reacted gas-phase product carries out carrying out condensation after the heat recuperation, obtains hydrochloric acid soln.Reacted fused salt carries out shrend, goes the carbonating tower carbonating.Carbonating finishes, solid-liquid separation, washing.Liquid phase KHCO
3Become K through thermolysis
2CO
3,, obtain K through evaporation concentration
2CO
3Product, solid phase becomes anhydrous potassium pentaborate through drying, returns the first step; Thermolysis gained carbon dioxide recovery is utilized;
Embodiment 1
Take by weighing 4mol KCl (analytical pure, content>=99.5%) and through 500 ℃ of dried 1mol KB
5O
8(by KOH and H
3BO
3Mix and produce), put into reactor drum after the mixing, be heated to 800 ℃ of fusions, feed 200 ℃ superheated vapour then, press 10mol quantity of steam design steam flow, reaction back condensed gas product obtains hydrochloric acid soln.Material after the fused salt Water Quenching is put into pressurized reactor, logical CO
2(content>=99%), at 0.1Mpa, 30 ℃ of following carbonation reactions 1 hour are cooled to 15 ℃ of crystallizations then; Pressure filtration, solid becomes KB in 500 ℃ of dryings
5O
8Recycle, filtrating is concentrated through heating, thermolysis, makes K
2CO
3, be weighed as 265g.
Embodiment 2
Take by weighing 4mol KCl (analytical pure, content>=99.5%) and through 500 ℃ of dried 1.1molKB
5O
8(by KOH and H
3BO
3Mix and produce), put into reactor drum after the mixing, be heated to 900 ℃ of fusions, feed 200 ℃ superheated vapour then, press 15mol quantity of steam design steam flow, reaction back condensed gas product obtains hydrochloric acid soln.Material after the fused salt Water Quenching is put into pressurized reactor, logical CO
2(content>=99%), at 0.1Mpa, 30 ℃ of following carbonation reaction 50min are cooled to 15 ℃ of crystallizations then; Pressure filtration, solid becomes KB in 500 ℃ of dryings
5O
8Recycle, filtrating is concentrated through heating, thermolysis, makes K
2CO
3, be weighed as 260g.
Embodiment 3
Take by weighing 4mol KCl (analytical pure, content>=99.5%) and through 500 ℃ of dried 1.1molKB
5O
8(by KOH and H
3BO
3Mix and produce), put into reactor drum after the mixing, be heated to 950 ℃ of fusions, feed 200 ℃ superheated vapour then, press 10mol quantity of steam design steam flow, reaction back condensed gas product obtains hydrochloric acid soln.Material after the fused salt Water Quenching is put into pressurized reactor, logical CO
2(content>=99%), at 0.1Mpa, 30 ℃ of following carbonation reaction 40min are cooled to 15 ℃ of crystallizations then; Pressure filtration, solid becomes KB in 500 ℃ of dryings
5O
8Recycle, filtrating is concentrated through heating, thermolysis, makes K
2CO
3, be weighed as 255g.
Claims (6)
1. a KCl melt hydrolysis method is directly produced the method for hydrochloric acid and salt of wormwood, it is characterized in that utilizing KB
5O
8Special property during molten state is with Repone K and KB
5O
8Melting mixing, 800～1200 ℃ of melt temperatures, mixing match KCl: KB
5O
8(4: 1～1.2) mol ratio, through hot water and steam, the hydrogen ion in the water combines with cl ions, becomes hydrogen chloride gas then, with reaction back remainder water steam, becomes hydrochloric acid soln after the condensation; The B that reaction generates
2O
3/ K
2The alkali metal borate that the ratio of O diminishes carries out shrend, then through carbonating post crystallization regeneration KB
5O
84H
2O recycles after drying; Carbonating obtains KHCO
3Solution obtains K through further handling
2CO
3
2. a kind of KCl melt hydrolysis method according to claim 1 is directly produced the method for hydrochloric acid and salt of wormwood; It is characterized in that described melt hydrolysis is under alkali metal chloride is in molten state; Feed superheated vapour, the hydrolysis reaction under the molten state is called " melt hydrolysis ".
3. a kind of KCl melt hydrolysis method according to claim 1 is directly produced the method for hydrochloric acid and salt of wormwood, it is characterized in that described KB
5O
8Special property during molten state is meant and is utilized in KB more than 800 ℃
5O
8Have acidity after the fusion, can sour environment be provided for the decomposition of KCl.
4. directly produce the method for hydrochloric acid and salt of wormwood according to the described a kind of KCl melt hydrolysis method of claim 1, it is characterized in that described superheated vapour is that temperature reaches more than 200 ℃, but pressure is non-pressurized superheated vapour.
5. a kind of KCl melt hydrolysis method according to claim 1 is directly produced the method for hydrochloric acid and salt of wormwood, it is characterized in that the B that described reaction generates
2O
3/ K
2The alkali metal borate that the ratio of O diminishes comprises B
2O
3/ K
2The ratio of O is a borate less than 2 serial K, is mainly K
2B
4O
7
6. a kind of KCl melt hydrolysis method according to claim 1 is directly produced the method for hydrochloric acid and salt of wormwood, it is characterized in that described carbonating post crystallization regeneration KB
5O
84H
2O, the carbonation reaction temperature is 30～40 ℃, pressure 0.1～0.3Mpa, Tc is 10～15 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112390229A (en) * | 2019-08-14 | 2021-02-23 | 骆曦明 | Method for preparing hydrochloric acid and potassium carbonate by taking potassium chloride as raw material |
| CN113600010A (en) * | 2021-07-19 | 2021-11-05 | 陕西未来能源化工有限公司 | Purification and regeneration method of hot potash solution in Fischer-Tropsch synthesis tail gas, device and application thereof |
-
2010
- 2010-11-25 CN CN2010105656292A patent/CN102476790A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《中国科学院过程工程研究所博士论文》 20061231 杨刚 ""碱金属氯化物熔态水解法联产盐酸与碳碱" 盐酸制备原理与工艺研究" 第1章、第5章 1-6 , * |
| 杨刚: """碱金属氯化物熔态水解法联产盐酸与碳碱" 盐酸制备原理与工艺研究"", 《中国科学院过程工程研究所博士论文》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112390229A (en) * | 2019-08-14 | 2021-02-23 | 骆曦明 | Method for preparing hydrochloric acid and potassium carbonate by taking potassium chloride as raw material |
| CN113600010A (en) * | 2021-07-19 | 2021-11-05 | 陕西未来能源化工有限公司 | Purification and regeneration method of hot potash solution in Fischer-Tropsch synthesis tail gas, device and application thereof |
| CN113600010B (en) * | 2021-07-19 | 2023-09-01 | 陕西未来能源化工有限公司 | Purification and regeneration method for Fischer-Tropsch synthesis tail gas hot potash solution, device and application thereof |
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Application publication date: 20120530 |