CN113730954A - Method for recovering isooctanol and sulfonated kerosene from waste organic of naphthenic acid system for extracting and separating yttrium - Google Patents
Method for recovering isooctanol and sulfonated kerosene from waste organic of naphthenic acid system for extracting and separating yttrium Download PDFInfo
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- CN113730954A CN113730954A CN202111055993.9A CN202111055993A CN113730954A CN 113730954 A CN113730954 A CN 113730954A CN 202111055993 A CN202111055993 A CN 202111055993A CN 113730954 A CN113730954 A CN 113730954A
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- isooctanol
- naphthenic acid
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- sulfonated kerosene
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- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 title claims abstract description 79
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000003350 kerosene Substances 0.000 title claims abstract description 51
- 229910052727 yttrium Inorganic materials 0.000 title claims abstract description 38
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000002699 waste material Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000004821 distillation Methods 0.000 claims abstract description 44
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 150000007524 organic acids Chemical class 0.000 claims abstract description 17
- 239000005416 organic matter Substances 0.000 claims abstract description 17
- 239000003513 alkali Substances 0.000 claims abstract description 16
- 238000007127 saponification reaction Methods 0.000 claims abstract description 13
- 238000004064 recycling Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 11
- 125000005609 naphthenate group Chemical group 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 5
- 239000002356 single layer Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims 1
- 230000008859 change Effects 0.000 abstract description 3
- 239000002253 acid Substances 0.000 description 20
- 239000002920 hazardous waste Substances 0.000 description 11
- 235000011121 sodium hydroxide Nutrition 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 238000000605 extraction Methods 0.000 description 5
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 5
- 239000012074 organic phase Substances 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 125000005608 naphthenic acid group Chemical group 0.000 description 3
- 238000012797 qualification Methods 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000010815 organic waste Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 naphthenic acid organic acid Chemical class 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010888 waste organic solvent Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for recovering isooctanol and sulfonated kerosene from waste organic matters of a naphthenic acid system for extracting and separating yttrium, which comprises the following steps: (1) taking scrapped organic of a naphthenic acid system for extracting and separating yttrium, wherein the initial organic acid value is 0.3-0.4mol/L, and mixing the scrapped organic with a saponified alkali liquor, wherein the saponification degree of the saponified alkali liquor on naphthenic acid is 150-300%; (2) placing the discarded organic matter treated in the step (1) in distillation equipment with the vacuum degree of-0.090 MPa to-0.100 MPa and the distillation temperature of 40 ℃ to 200 ℃ to evaporate a mixture of isooctanol and sulfonated kerosene; (3) recycling the mixture of the isooctanol and the sulfonated kerosene; the invention can recycle the mixture of kerosene and isooctanol in the discarded organic of naphthenic acid system for extracting and separating yttrium at low cost, reduce the generation amount of dangerous waste (reduce the amount of the dangerous waste), and change waste into valuable.
Description
Technical Field
The invention relates to the technical field of rare earth extraction and separation, in particular to a method for recovering isooctyl alcohol and sulfonated kerosene from waste organic of a naphthenic acid system for extracting and separating yttrium.
Background
The rare earth extraction separation yttrium usually uses a naphthenic acid extraction system, the organic phase of the naphthenic acid extraction system comprises naphthenic acid, sulfonated kerosene and isooctyl alcohol, and the content of the naphthenic acid is about 20 percent. The acid value of the newly prepared organic phase is about 0.60mol/L, the acid value of the organic phase gradually decreases along with the operation of the production process, when the acid value is lower than 0.40mol/L, the organic phase can not maintain stable production, and the organic waste becomes hazardous waste (hazardous waste categories are: HW06 waste organic solvent and organic solvent-containing waste, hazardous waste code: 900-. In recent years, with the popularization of hydro-oxidation methods in the petrochemical industry, the raw material crude acid for preparing naphthenic acid is less and less, the quality of the naphthenic acid is poorer and poorer, the reduction speed of the organic acid value is accelerated, and the amount of hazardous waste generated each year is doubled.
The existing organic scrap treatment mode is sold to a company with the treatment qualification of hazardous wastes as hazardous wastes, and is used for manufacturing building materials such as bricks, asphalt and the like.
The known near-scrap organic method is mainly a method for preparing or refining naphthenic acid, in particular to refining crude naphthenic acid or low-acid-value naphthenic acid into high-acid-value naphthenic acid.
Chinese patent CN 1058986a discloses a method for separating unsaponifiable matter in naphthenic acid, which is to saponify crude naphthenic acid containing 10-55% of unsaponifiable matter, then directly distill under reduced pressure (temperature is above 300 ℃) to separate unsaponifiable matter, and acidify the rest naphthenic acid soap at high temperature to obtain acidified naphthenic acid with crude acid value of more than 195 mgKOH/g. The method aims to remove unsaponifiable substances to prepare naphthenic acid with high acid value, and has the defect that the distillation temperature exceeds 280 ℃ and the energy consumption is high.
The refining method of naphthenic acid disclosed in chinese patent CN 1101340a is that crude naphthenic acid or two or three-stage low acid value naphthenic acid is saponified, then solvent oil, gasoline or kerosene is used as extractant to extract and separate unsaponifiable matter in the saponified solution, the separated water phase is acidified and washed, finally the residual extractant is distilled under reduced pressure at 200 ℃ to obtain 100% of first-stage naphthenic acid. The method aims at purifying naphthenic acid, and has the defects of complex flow and complicated operation. The new process for preparing high acid value by using low acid value naphthenic acid disclosed in Chinese patent CN 1068323A is characterized by that the tertiary naphthenic acid (low acid value naphthenic acid or lower acid value naphthenic acid) is added into a certain quantity of light diesel oil or kerosene to dilute, then a certain quantity of 5% NaOH solution is added, and the above-mentioned materials are saponified, acidified and distilled under reduced pressure to obtain primary and secondary naphthenic acids (high acid value naphthenic acid). The method aims to prepare the naphthenic acid with high acid value from the naphthenic acid with low acid value, and has the defects of complex flow and fussy operation. In summary, the current organic treatment methods for discarding naphthenic acid systems used for extracting and separating yttrium focus on refining crude naphthenic acid or low acid value naphthenic acid into high acid value naphthenic acid, and isooctanol and sulfonated kerosene in the discarded organic of naphthenic acid systems used for extracting and separating yttrium continue to exist as hazardous wastes.
Disclosure of Invention
The invention aims to provide a method for recovering isooctanol and sulfonated kerosene from waste organic of a naphthenic acid system for extracting and separating yttrium, which can recover kerosene and isooctanol mixture in the waste organic of the naphthenic acid system for extracting and separating yttrium at low cost, reduce the generation amount of dangerous waste (reduce the amount of the dangerous waste) and change waste into valuable.
In order to achieve the purpose, the technical solution of the invention is as follows:
a process for recovering isooctanol and sulfonated kerosene from waste organic streams of naphthenic acid systems for the extractive separation of yttrium, comprising the steps of: (1) taking scrapped organic of a naphthenic acid system for extracting and separating yttrium, wherein the initial organic acid value is 0.3-0.4mol/L, and mixing the scrapped organic with a saponified alkali liquor, wherein the saponification degree of the saponified alkali liquor on naphthenic acid is 150-300%; (2) placing the discarded organic matter treated in the step (1) in distillation equipment with the vacuum degree of-0.090 MPa to-0.100 MPa and the distillation temperature of 40 ℃ to 200 ℃ to evaporate a mixture of isooctanol and sulfonated kerosene; (3) and (4) recycling the mixture of the isooctanol and the sulfonated kerosene.
The distillation time is 14-66 h.
The distillation temperature is increased from 40 ℃, and the temperature increasing speed is 5 ℃/2-10 ℃/h.
The alkali in the saponified alkali solution is any one of sodium hydroxide, calcium hydroxide or potassium hydroxide.
The distillation equipment is any one of a rotary evaporator, a single-layer glass reaction kettle or a stainless steel reaction kettle.
The vacuum degree is controlled by a vacuum pump.
The vacuum pump is any one of a circulating water vacuum pump, a water injection vacuum pump or a reciprocating pump.
And (4) recycling the isooctanol and sulfonated kerosene mixture distilled in the step (3) to a naphthenic acid system and a P07 alcohol system for extracting and separating yttrium.
The raffinate formed in step (2) is naphthenate.
After the technical scheme is adopted, the waste organic of the naphthenic acid system for extracting and separating yttrium is saponified by using the saponification alkali liquor before distillation, so that naphthenic acid in the waste organic is converted into naphthenate and water, and then the water, isooctanol and sulfonated kerosene are vaporized by controlling the distillation temperature and the vacuum degree to distill, so that isooctanol and sulfonated kerosene are separated from the waste organic and are recycled.
Detailed Description
To achieve the above objects and advantages, the present invention provides a novel and improved technical means and structure, which will be described in detail in connection with the preferred embodiments of the present invention.
At normal temperature, the boiling points of all components in the scrapped organic of the naphthenic acid system for extracting and separating yttrium are respectively as follows: naphthenic acid 210-420 ℃, isooctanol 171 ℃ and sulfonated kerosene 180-260 ℃, and the boiling point of naphthenate is far higher than that of naphthenic acid.
The invention discloses a method for recovering isooctanol and sulfonated kerosene from waste organic of naphthenic acid system for extracting and separating yttrium, which comprises the following steps: (1) taking scrapped organic of a naphthenic acid system for extracting and separating yttrium, wherein the initial organic acid value is 0.3-0.4mol/L, and mixing the scrapped organic with a saponified alkali liquor, wherein the saponification degree of the saponified alkali liquor on naphthenic acid is 150-300%; (2) placing the discarded organic matter treated in the step (1) in distillation equipment with the vacuum degree of-0.090 MPa to-0.100 MPa and the distillation temperature of 40 ℃ to 200 ℃ to evaporate a mixture of isooctanol and sulfonated kerosene; (3) and (4) recycling the mixture of the isooctanol and the sulfonated kerosene. Wherein the saponification degree is calculated as "concentration of saponified lye × (volume of saponified lye/(volume of organic acid value) × 100%.
Through a plurality of experimental tests, the following results are obtained: if the vacuum degree is lower than-0.090 MPa, the distillation temperature needs to be increased to more than 50 ℃ to achieve the same effect, and the low-temperature distillation effect cannot be achieved; if the vacuum degree is higher than-0.100 MPa, the distillation process is easy to explode, the distillation time needs to be greatly prolonged for avoiding the explosion, and the distillation efficiency is reduced; if nothing is distilled out at a temperature lower than 40 ℃, if the residue begins to be semi-solidified after being higher than 200 ℃, almost no matter is distilled out again or even if the residue can be distilled out, the residue after being distilled out is not easy to process due to excessive viscosity and poor liquidity.
Further, the isooctanol and sulfonated kerosene mixture distilled out in the step (3) is recycled to a naphthenic acid system and a P07 alcohol system for extracting and separating yttrium.
Wherein, the distillation time can be 14-66 h; the distillation temperature can be increased from 40 ℃, and the temperature increasing speed is 5 ℃/2 h-10 ℃/h; through a plurality of experimental tests, the following results are obtained: if the temperature rise speed is too high, the temperature rise speed is explosive, the temperature rise speed is too low, the distillation time is long, the distillation efficiency is low, and the treatment capacity is small.
The alkali in the saponified lye can be any of sodium hydroxide, calcium hydroxide or potassium hydroxide.
Next, the distillation apparatus may be any one of a rotary evaporator, a single-layer glass reaction vessel, or a stainless steel reaction vessel.
Further, the vacuum degree is controlled by a vacuum pump; the vacuum pump can be any one of a circulating water vacuum pump, a water injection vacuum pump or a reciprocating pump.
Further, the raffinate formed in step (2) is naphthenate.
In conclusion, the waste organic of the naphthenic acid system for extracting and separating yttrium is saponified by using the saponified alkali liquor before distillation, so that naphthenic acid in the waste organic is converted into naphthenate and water, and then the water, isooctanol and sulfonated kerosene are gasified by controlling proper distillation temperature and vacuum degree to distill, thereby realizing the separation of isooctanol and sulfonated kerosene from the waste organic for recycling, therefore, the invention can recycle the mixture of kerosene and isooctanol in the waste organic of the naphthenic acid system for extracting and separating yttrium at low cost, reduce the generation amount of hazardous waste (reduce hazardous waste), and change waste into valuable; in the steps of the method, the boiling point of each component is reduced by applying negative pressure, so that water, isooctanol and sulfonated kerosene can be vaporized at a lower temperature; and the vaporized water, isooctanol and sulfonated kerosene can be cooled and liquefied by a condensing device, the water in the obtained liquid is in the lower layer, and the mixture of isooctanol and sulfonated kerosene is in the upper layer.
Example 1
400mL of discarded organic of naphthenic acid system for extracting and separating yttrium is taken, the initial organic acid value is 0.38mol/L, the discarded organic is fully mixed with 40mL of NaOH solution with the concentration of 10.8mol/L (the saponification degree is 284%), and then the mixture is placed in a 1L rotary evaporator for reduced pressure distillation, the rotating speed is 10rpm, the vacuum degree is-0.096 MPa, the heating speed is 10 ℃/2h, the maximum distillation temperature is 180 ℃, and the total distillation time is 30 hours. 255mL of organic solvent was distilled off, and the organic acid value was less than 0.01mol/L, resulting in a yield of 63.75%. The content of isooctyl alcohol in the distilled organic is about 45.5 percent by NMR/GC-MS detection; the distilled organic matter is the mixture of isooctanol and kerosene, and can be recovered for preparing new organic matter.
Since the pure naphthenic acid organic acid value is about 3.0mol/L, 400mL of organic acid with 0.38mol/L acid value theoretically contains: naphthenic acid-400 x 0.38/3=50.67mL, isooctanol and sulfonated kerosene mixture-400-50.67 =349.33 mL. 349.33mL can be distilled out theoretically, but because saponification is carried out before distillation, naphthenic acid is converted into naphthenate, and the viscosity is increased remarkably, the residue is semi-solidified when 255mL is distilled out, if further distillation is carried out, the temperature needs to be increased remarkably, and the residue is not easy to treat.
The method ensures that naphthenic acid is not distilled out completely through saponification, and ensures that distilled organic matter has more isooctyl alcohol and kerosene.
Example 2
400mL of the waste organic of naphthenic acid system used for extracting and separating yttrium are taken, the initial organic acid value is 0.40mol/L, and 50mL of Ca (OH) with the concentration of 6.2mol/L2After the solution was sufficiently mixed (degree of saponification: 194%), the mixture was distilled under reduced pressure in a 1L rotary evaporator at a rotation speed of 10rpm, a vacuum degree of-0.095 MPa, a temperature rise rate of 5 ℃/2h, a maximum distillation temperature of 170 ℃ for a total of 54 hours. 235mL of organic matter is distilled out, the organic acid value is less than 0.01mol/L, and the yield is 58.75%. The content of isooctyl alcohol in the distilled organic is about 47.2 percent by NMR/GC-MS detection; the distilled organic matter is the mixture of isooctanol and kerosene, and can be recovered for preparing new organic matter.
Example 3
10L of scrapped organic of naphthenic acid system for extracting and separating yttrium is taken, the initial organic acid value is 0.37mol/L, the scrapped organic is fully mixed with 0.8L of NaOH solution and 10.8mol/L of NaOH solution (the saponification degree is 234 percent), and then the mixture is placed in a 30L single-layer glass reaction kettle for reduced pressure distillation, the vacuum degree is-0.099 MPa, the temperature rise speed is 5 ℃/2h, the maximum distillation temperature is 170 ℃, and the total distillation time is 54 hours. 6.62L of the organic phase was distilled off, the organic acid value was less than 0.01mol/L, and the yield was 66.2%. The content of isooctyl alcohol in the distilled organic is about 39.8 percent by NMR/GC-MS detection; the distilled organic matter is the mixture of isooctanol and kerosene, and can be recovered for preparing new organic matter.
Example 4
Taking 10L of discarded organic of naphthenic acid system for extracting and separating yttrium, wherein the initial organic acid value is 0.41mol/L, and mixing the discarded organic with 1.2L of Ca (OH) of 6.2mol/L2After the solution is fully mixed (the saponification degree is 181%), the mixture is placed in a 30L single-layer glass reaction kettle for reduced pressure distillation, the vacuum degree is minus 0.099MPa, the temperature rise speed is 10 ℃/h, the maximum distillation temperature is 190 ℃, and the total distillation time is 16 hours. 6.05L of organic matter is distilled out, the organic acid value is less than 0.01mol/L, and the yield is 60.5%. The content of isooctyl alcohol in the distilled organic is about 42.8 percent by NMR/GC-MS detection; the distilled organic matter is the mixture of isooctanol and kerosene, and can be recovered for preparing new organic matter.
Example 5
Take 2m3The discarded organic of naphthenic acid system for extracting and separating yttrium, the initial organic acid value is 0.36mol/L, after fully mixing with 0.15L, 10.8mol/L NaOH solution (saponification degree is 225%), placing at 5m3The vacuum distillation is carried out in a stainless steel reaction kettle, the vacuum degree is minus 0.094MPa, the temperature rise speed is 5 ℃/h, the maximum distillation temperature is 180 ℃, and the total distillation time is 29 hours. The organic layer was distilled off to 1.12m3The organic acid value is less than 0.01mol/L, and the yield is 56.0%. The content of isooctyl alcohol in the distilled organic is about 53.3 percent by NMR/GC-MS detection; (ii) a The distilled organic matter is the mixture of isooctanol and kerosene, and can be recovered for preparing new organic matter.
Naphthenic acid systems used for the extractive separation of yttrium usually have periodic additions of isooctanol and naphthenic acid due to a decrease in acid number, which results in the isooctanol content in the rejected organic being usually higher than 20% of the original formulation, plus the boiling point of isooctanol being lower than that of sulfonated kerosene, both of which result in the isooctanol content in the distilled organic being above 30%. Therefore, the distilled organic can be used as new organic of a naphthenic acid system and a P507 alcohol system which are prepared again and used for extracting and separating yttrium, and the new organic can be reused in an extraction production line. The residue is treated according to the prior hazardous waste treatment method. The organic evaporation yield of the invention is more than 50 percent, which means that more than half of hazardous waste can be reduced, and the organic evaporation is reused for preparing new organic, thus changing waste into valuable, saving the cost of purchasing part of isooctanol and sulfonated kerosene, and having considerable economic benefit and obvious environmental protection effect.
Wherein, the majority of the residue after the treatment of the invention is naphthenate, and a small amount of impurities such as modified naphthenic acid, etc. The distillation residue needs to be ensured to be treated according to the existing organic treatment mode of naphthenic acid scrap, and the control condition is a key point of the technical control of the invention, so that the distillation residue cannot be excessively distilled to cause high viscosity. As mentioned above, most of the existing organic waste disposal methods are sold to companies with dangerous waste disposal qualification for manufacturing building materials such as bricks, asphalt and the like. The scrapped naphthenic acid from these companies is mainly viscosity and acid-base property, and firstly, the viscosity cannot be too high, and the pump can be used for pumping and stirring; secondly, the organic matters cannot be acidic, so that the waste organic matters are required to be adjusted to be alkaline by lime, liquid alkali and the like before being sold. So that substantially naphthenates are also obtained. The residue obtained by the method is naphthenate, and can be directly purchased to companies with related treatment qualification without adding lime or liquid caustic soda for neutralization.
While the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention. Therefore, the scope of the present invention should not be limited to the embodiments disclosed, but includes various alternatives and modifications without departing from the present invention, which are encompassed by the claims.
Claims (9)
1. A method for recovering isooctanol and sulfonated kerosene from waste organic of naphthenic acid system for extracting and separating yttrium, which is characterized by comprising the following steps:
(1) taking scrapped organic of a naphthenic acid system for extracting and separating yttrium, wherein the initial organic acid value is 0.3-0.4mol/L, and mixing the scrapped organic with a saponified alkali liquor, wherein the saponification degree of the saponified alkali liquor on naphthenic acid is 150-300%;
(2) placing the discarded organic matter treated in the step (1) in distillation equipment with the vacuum degree of-0.090 MPa to-0.100 MPa and the distillation temperature of 40 ℃ to 200 ℃ to evaporate a mixture of isooctanol and sulfonated kerosene;
(3) and (4) recycling the mixture of the isooctanol and the sulfonated kerosene.
2. The method for recovering isooctanol and sulfonated kerosene according to claim 1 from waste organic of naphthenic acid system for extracting and separating yttrium, wherein: the distillation time is 14-66 h.
3. A process according to claim 1 or 2 for the recovery of isooctanols and sulfonated kerosene from spent organics of naphthenic acid systems for the extractive separation of yttrium, characterized in that: the distillation temperature is increased from 40 ℃, and the temperature increasing speed is 5 ℃/2-10 ℃/h.
4. The method for recovering isooctanol and sulfonated kerosene according to claim 1 from waste organic of naphthenic acid system for extracting and separating yttrium, wherein: the alkali in the saponified alkali solution is any one of sodium hydroxide, calcium hydroxide or potassium hydroxide.
5. The method for recovering isooctanol and sulfonated kerosene according to claim 1 from waste organic of naphthenic acid system for extracting and separating yttrium, wherein: the distillation equipment is any one of a rotary evaporator, a single-layer glass reaction kettle or a stainless steel reaction kettle.
6. The method for recovering isooctanol and sulfonated kerosene according to claim 1 from waste organic of naphthenic acid system for extracting and separating yttrium, wherein: the vacuum degree is controlled by a vacuum pump.
7. The method for recovering isooctanol and sulfonated kerosene according to claim 6, wherein said method comprises the steps of: the vacuum pump is any one of a circulating water vacuum pump, a water injection vacuum pump or a reciprocating pump.
8. The method for recovering isooctanol and sulfonated kerosene according to claim 1 from waste organic of naphthenic acid system for extracting and separating yttrium, wherein: and (4) recycling the isooctanol and sulfonated kerosene mixture distilled in the step (3) to a naphthenic acid system and a P07 alcohol system for extracting and separating yttrium.
9. The method for recovering isooctanol and sulfonated kerosene according to claim 1 from waste organic of naphthenic acid system for extracting and separating yttrium, wherein: the raffinate formed in step (2) is naphthenate.
Priority Applications (1)
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Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB781578A (en) * | 1954-04-23 | 1957-08-21 | Universal Oil Company Ltd | Improvements relating to processes for the refining of naphthenic acids by distillation |
GB2053711A (en) * | 1979-07-10 | 1981-02-11 | Inst Neftekhim Protses Im Ju G | Catalyst for method of preparing naphthenic acids |
CN1058986A (en) * | 1990-08-16 | 1992-02-26 | 岳阳石油化工总厂研究院 | Process for separating unsaponifiable matter from naphthenic acid |
CN1101340A (en) * | 1993-10-06 | 1995-04-12 | 南开大学 | Refining process for naphthenic acid |
US5741925A (en) * | 1997-01-13 | 1998-04-21 | Air Products And Chemicals, Inc. | Transvinylation of naphthenic acids |
EP1911829A1 (en) * | 2006-10-10 | 2008-04-16 | The Queen's University of Belfast | Process for deacidifying crude oil |
US20100300937A1 (en) * | 2009-05-27 | 2010-12-02 | IP Services Group-ATTN: Docketing | Naphthenic acid removal and conversion |
CN107604162A (en) * | 2015-12-24 | 2018-01-19 | 广西师范大学 | A kind of mixed extractant for separating yttrium |
US20190093002A1 (en) * | 2018-11-21 | 2019-03-28 | Shell Oil Company | Hydrocarbon recovery composition and a method for use thereof |
CN110407686A (en) * | 2019-06-27 | 2019-11-05 | 五矿(北京)稀土研究院有限公司 | A method of the separating naphthenic acid from mixing organic matter |
CN112831656A (en) * | 2020-12-31 | 2021-05-25 | 广西国盛稀土新材料有限公司 | Method for regenerating naphthenic acid extraction organic phase |
CN113088692A (en) * | 2021-04-06 | 2021-07-09 | 鞍山昊旻稀土科技有限公司 | Extractant for extracting naphthenic acid and yttrium extraction process |
-
2021
- 2021-09-09 CN CN202111055993.9A patent/CN113730954A/en active Pending
Patent Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB781578A (en) * | 1954-04-23 | 1957-08-21 | Universal Oil Company Ltd | Improvements relating to processes for the refining of naphthenic acids by distillation |
GB2053711A (en) * | 1979-07-10 | 1981-02-11 | Inst Neftekhim Protses Im Ju G | Catalyst for method of preparing naphthenic acids |
CN1058986A (en) * | 1990-08-16 | 1992-02-26 | 岳阳石油化工总厂研究院 | Process for separating unsaponifiable matter from naphthenic acid |
CN1101340A (en) * | 1993-10-06 | 1995-04-12 | 南开大学 | Refining process for naphthenic acid |
US5741925A (en) * | 1997-01-13 | 1998-04-21 | Air Products And Chemicals, Inc. | Transvinylation of naphthenic acids |
EP1911829A1 (en) * | 2006-10-10 | 2008-04-16 | The Queen's University of Belfast | Process for deacidifying crude oil |
US20100300937A1 (en) * | 2009-05-27 | 2010-12-02 | IP Services Group-ATTN: Docketing | Naphthenic acid removal and conversion |
CN107604162A (en) * | 2015-12-24 | 2018-01-19 | 广西师范大学 | A kind of mixed extractant for separating yttrium |
US20190093002A1 (en) * | 2018-11-21 | 2019-03-28 | Shell Oil Company | Hydrocarbon recovery composition and a method for use thereof |
CN110407686A (en) * | 2019-06-27 | 2019-11-05 | 五矿(北京)稀土研究院有限公司 | A method of the separating naphthenic acid from mixing organic matter |
CN112831656A (en) * | 2020-12-31 | 2021-05-25 | 广西国盛稀土新材料有限公司 | Method for regenerating naphthenic acid extraction organic phase |
CN113088692A (en) * | 2021-04-06 | 2021-07-09 | 鞍山昊旻稀土科技有限公司 | Extractant for extracting naphthenic acid and yttrium extraction process |
Non-Patent Citations (3)
Title |
---|
刘公召等: "提高石油环烷酸质量的工艺研究", 《沈阳化工学院学报》 * |
曹逸飞等: "环烷酸及其盐类的应用研究", 《广东化工》 * |
杨启山等: "高纯氧化钇清洁化生产工艺的研究", 《稀土》 * |
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