CN101041421A - Method for industrial hydrochloric acid purification by liquid extraction - Google Patents
Method for industrial hydrochloric acid purification by liquid extraction Download PDFInfo
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- CN101041421A CN101041421A CN 200710027238 CN200710027238A CN101041421A CN 101041421 A CN101041421 A CN 101041421A CN 200710027238 CN200710027238 CN 200710027238 CN 200710027238 A CN200710027238 A CN 200710027238A CN 101041421 A CN101041421 A CN 101041421A
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- hydrochloric acid
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- liquid extraction
- acid purification
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a method of extractive purifying industrial alcaine, which comprises the following steps: setting triallylamine as extractant, isooctanol as assisting solvent and coal oil as diluent; forming extract organic phase through kerosene; extracting industrial alcaine in the extract pot; washing through pure water; stripping; getting high-purity alcaine. The invention possesses steady quality and high-purity, which can realize continuous mass production.
Description
Technical field
The invention belongs to field of fine chemical, relate to the method that a kind of technical hydrochloric acid is purified.
Background technology
The main method of technical hydrochloric acid purification at present has distillation method and resin method.Distillation method is with the technical hydrochloric acid heating evaporation, and the hydrogen chloride gas that steams obtains high purity hydrochloric acid through condensation or absorption, and its shortcoming is that energy consumption is big, and the maintenance of the equipment difficulty is big, poor stability, work under bad environment, production efficiency is low, the cost height, unstable product quality can not continuous production.Resin method is by the high molecular functional polymeric adsorbent with technical hydrochloric acid, the dianion absorption of the metal ion that exists in the technical hydrochloric acid and some amount is removed, its disadvantage is to remove light metal ion weak effect, do not reach some to the service requirements that Ca, Mg have relatively high expectations, influenced its use range.
Summary of the invention
It is good that purpose of the present invention has just provided a kind of safety performance, and constant product quality can realize the method for the industrial hydrochloric acid purification by liquid extraction of automatization control.
Principles of Chemical Engineering of the present invention are: trialkylamine code name N235 can extract acid and form ammonium salt, can also extract excess acid after forming ammonium salt, under high acidity, metal ions such as trialkylamine energy extracting Cu, Zn, Fe, Co, Cd, Bi, it extracts complex ability greater than extraction H ion, and does not extract Pb, Ni and alkalimetal ion and alkaline-earth metal ions substantially.Trialkylamine extraction acid and metal ion are realized with the coulombic force effect, so promptly the acid and the metal ion back extraction of extraction can be got off with the very little water of polarity.
The technical solution adopted in the present invention is: with trialkylamine code name N235 is that extraction agent, isooctyl alcohol code name ROH are that solubility promoter, kerosene are that thinner is formed extracted organic phase, extracts technical hydrochloric acid in extraction tank, through pure water washing, back extraction, obtains high purity hydrochloric acid.
Described extracted organic phase volume ratio is 10～30% trialkylamines, 10～30% isooctyl alcohol, all the other are kerosene.
Described extracted organic phase: technical hydrochloric acid: the pure water flow is 60～100: 15～25: 6～10.
18～23 grades of the total progression of described extraction tank, progression are configured to 3～5 grades of extraction sections, 2～3 grades of settling sections, 3～5 grades of washing sections, 5～10 grades of stripping sections.
Described extracted organic phase enters for the 1st grade from extraction tank, and technical hydrochloric acid enters from extraction tank the 2nd～5 fraction 2～3, and pure water is from the 18th～23 grade of adding of extraction tank, and high purity hydrochloric acid is drawn for the 8th～14 grade from extraction tank.
Described extraction section is provided with steam and heats, and makes 35～45 ℃ of the interior solution temperatures of extraction tank.
Described washing section and stripping section are provided with adjustable water internal circulation apparatus.
The 15th～20 grade of stripping section of described extraction tank offered spent acid outlet, and by high purity hydrochloric acid: the spent acid flow is 2～3.5: 0.2～0.4, and Cu, Zn, Fe, Co, Cd, the Bi impurity that makes the trialkylamine extraction is drawn by after the water back extraction time.
The present invention can realize serialization scale operation, constant product quality, and the purity height, easy and simple to handle, environmental pollution is little, and security is good, and cost for purification is low, and as cooperating flow control technique and relevant device, technological process can realize automatization control.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but it is not represented as unique embodiment of the present invention.
Embodiment one
Get 10%N235,10%ROH, 80% kerosene composition extracted organic phase by volume, technical hydrochloric acid concentration: 9.86N, CaO 39.25mg/L, Fe
2O
30.069mg/L, PbO 0.32mg/L, ZnO 0.5mg/L, NiO 0.019mg/L, CuO 0.044mg/L, CaO, Fe in the pure water
2O
3, PbO, ZnO, NiO, CuO be all less than 0.01mg/L; 18 grades of the total progression of adverse current mixed settler extractor, progression are configured to 3 grades of extraction sections, 2 grades of settling sections, 4 grades of washing sections, 9 grades of stripping sections.Extracted organic phase enters for the 1st grade from the adverse current mixed settler extractor, technical hydrochloric acid enters for the 2nd, 3 grades from the adverse current mixed settler extractor, pure water enters extracted organic phase for the 18th grade from the adverse current mixed settler extractor: technical hydrochloric acid: the pure water flow is 60L/min: 15L/min: 6L/min.Technical hydrochloric acid divides enter the adverse current mixed settler extractor and contact with extracted organic phase at 2, can effectively improve the collection acid amount of N235, and high purity hydrochloric acid concentration is improved.Be provided with 2 grades of settling sections after the extraction section, can guarantee that the two-phase phase-splitting is clear, avoid because extracted organic phase is carried Ca in the technical hydrochloric acid secretly
2+, Mg
2+And cause Ca in the high purity hydrochloric acid
2+, Mg
2+Raise.Extraction section is provided with steam and heats, and making interior solution of adverse current mixed settler extractor such as extracted organic phase, technical hydrochloric acid equitemperature is 35 ℃, effectively improves two-phase and divides phase effect, reduces because extracted organic phase is carried Ca in the technical hydrochloric acid secretly
2+, Mg
2+And cause high purity hydrochloric acid Ca
2+, Mg
2+Raise.Washing section and stripping section are provided with adjustable water internal circulation apparatus, reduce the amount of water of washing, back extraction, improve high purity hydrochloric acid concentration, but guarantee washing, strip aqueous amount and extracted organic phase amount ratio is unlikely differs too big, and cause washing, the decline of back extraction effect to make the high purity hydrochloric acid downgrade.Offer corresponding outlet the 1st grade of adverse current mixed settler extractor, the 8th grade and the 15th grade, draw and obtain raffinate, high purity hydrochloric acid and spent acid, high purity hydrochloric acid: the spent acid flow is 2L/min: 0.2L/min, offer the spent acid outlet at adverse current mixed settler extractor stripping section, Cu, Zn, Fe, Co, Cd, the Bi impurity of trialkylamine extraction are drawn after under the water back extraction, thereby do not enter high purity hydrochloric acid, guarantee the high purity hydrochloric acid quality.Raffinate and spent acid merging are used in addition as technical hydrochloric acid.
Detect by analysis: high purity hydrochloric acid concentration is 7.88N, CaO 0.5mg/L, PbO 0.09mg/L, ZnO 0.01mg/L, NiO＜0.01mg/L, CuO 0.023mg/L, has reached analytical pure impurity standard.
Embodiment two
Get 30%N235,30%ROH, 40% kerosene composition extracted organic phase by volume, technical hydrochloric acid concentration: 9.92N, CaO 45.36mg/L, Fe
2O
30.18mg/L, PbO 0.36mg/L, ZnO 0.44mg/L, NiO 0.021mg/L, CuO 0.038mg/L, CaO, Fe in the pure water
2O
3, PbO, ZnO, NiO, CuO be all less than 0.01mg/L; 23 grades of the total progression of adverse current mixed settler extractor, progression are configured to 5 grades of extraction sections, 3 grades of settling sections, 5 grades of washing sections, 10 grades of stripping sections.Extracted organic phase enters for the 1st grade from the adverse current mixed settler extractor, technical hydrochloric acid enters from 3 of adverse current mixed settler extractor the 3rd, 4,5 fractions, pure water enters extracted organic phase for the 20th grade from the adverse current mixed settler extractor: technical hydrochloric acid: the pure water flow is 100L/min: 25L/min: 10L/min.Be provided with 3 grades of settling sections after the extraction section.Extraction section is provided with steam and heats, and makes 45 ℃ of the interior solution temperatures of adverse current mixed settler extractor.Washing section and stripping section are provided with adjustable water internal circulation apparatus.Offer corresponding outlet the 1st grade of adverse current mixed settler extractor, the 14th grade and the 20th grade, draw and obtain raffinate, high purity hydrochloric acid and spent acid, high purity hydrochloric acid: the spent acid flow is 3.5L/min: 0.4L/min, and raffinate and spent acid merging are used in addition as technical hydrochloric acid.
Detect by analysis: high purity hydrochloric acid concentration is 8.23N, CaO 0.36mg/L, PbO 0.074mg/L, ZnO 0.01mg/L, NiO＜0.01mg/L, CuO 0.018mg/L, has reached analytical pure impurity standard.
Claims (8)
1, a kind of method of industrial hydrochloric acid purification by liquid extraction is characterized in that with the trialkylamine being that extraction agent, isooctyl alcohol are that solubility promoter, kerosene are that thinner is formed extracted organic phase, extracts technical hydrochloric acid in extraction tank, through pure water washing, back extraction, obtains high purity hydrochloric acid.
2, the method for industrial hydrochloric acid purification by liquid extraction according to claim 1 is characterized in that described extracted organic phase volume ratio is 10～30% trialkylamines, 10～30% isooctyl alcohol, all the other are kerosene.
3, the method for industrial hydrochloric acid purification by liquid extraction according to claim 1 is characterized in that described extracted organic phase: technical hydrochloric acid: the pure water flow is 60～100: 15～25: 6～10.
4, the method for industrial hydrochloric acid purification by liquid extraction according to claim 1 is characterized in that 18～23 grades of the total progression of described extraction tank, and progression is configured to 3～5 grades of extraction sections, 2～3 grades of settling sections, 3～5 grades of washing sections, 5～10 grades of stripping sections.
5, the method for industrial hydrochloric acid purification by liquid extraction according to claim 1, it is characterized in that described extracted organic phase enters for the 1st grade from extraction tank, technical hydrochloric acid enters from extraction tank the 2nd～5 fraction 2～3, pure water is from the 18th～23 grade of adding of extraction tank, and high purity hydrochloric acid is drawn for the 8th～14 grade from extraction tank.
6, the method for industrial hydrochloric acid purification by liquid extraction according to claim 4 is characterized in that described extraction section is provided with steam and heats, and makes 35～45 ℃ of the interior solution temperatures of extraction tank.
7, the method for industrial hydrochloric acid purification by liquid extraction according to claim 4 is characterized in that described washing section and stripping section are provided with adjustable water internal circulation apparatus.
8, the method for industrial hydrochloric acid purification by liquid extraction according to claim 4 is characterized in that the 15th～20 grade of stripping section of described extraction tank offer spent acid outlet, and high purity hydrochloric acid: the spent acid flow is 2～3.5: 0.2～0.4.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710027238 CN101041421A (en) | 2007-03-22 | 2007-03-22 | Method for industrial hydrochloric acid purification by liquid extraction |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710027238 CN101041421A (en) | 2007-03-22 | 2007-03-22 | Method for industrial hydrochloric acid purification by liquid extraction |
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Family
ID=38807252
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|---|---|---|---|
| CN 200710027238 Pending CN101041421A (en) | 2007-03-22 | 2007-03-22 | Method for industrial hydrochloric acid purification by liquid extraction |
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| US8106246B2 (en) | 2005-11-08 | 2012-01-31 | Solvay (Societe Anonyme) | Process for the manufacture of dichloropropanol by chlorination of glycerol |
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