CN112940781B - Diluent and preparation and application thereof - Google Patents

Diluent and preparation and application thereof Download PDF

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Publication number
CN112940781B
CN112940781B CN201911254515.3A CN201911254515A CN112940781B CN 112940781 B CN112940781 B CN 112940781B CN 201911254515 A CN201911254515 A CN 201911254515A CN 112940781 B CN112940781 B CN 112940781B
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diluent
fraction
sapo
extraction
temperature
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CN112940781A (en
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丛昱
唐南方
商庆浩
陈帅
吴春田
许国梁
苏哲
何辉
袁洁琼
曹智
王文涛
谢书宝
罗方祥
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Dalian Institute of Chemical Physics of CAS
China Institute of Atomic of Energy
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Dalian Institute of Chemical Physics of CAS
China Institute of Atomic of Energy
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
    • C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02—Obtaining thorium, uranium, or other actinides
    • C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
    • C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
    • C22B60/026—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries liquid-liquid extraction with or without dissolution in organic solvents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02—Obtaining thorium, uranium, or other actinides
    • C22B60/04—Obtaining plutonium
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/1022—Fischer-Tropsch products
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/70—Catalyst aspects
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies

Abstract

The invention relates to a preparation method of a diluent. The method mainly comprises the following steps: fischer-Tropsch distillate oil and hydrogen are taken as raw materials, pt/SAPO-11@ beta is taken as a catalyst, the reaction pressure is 1.0MPa to 4.0MPa, the reaction temperature is 250 ℃ to 400 ℃, and the airspeed is 0.5h ‑1 ‑3h ‑1 And the hydrogen-oil ratio is 600. And then, rectifying the generated isoparaffin to separate out middle fraction, thus obtaining the target diluent. The prepared diluent is used for a spent fuel extractant and can selectively extract and separate uranium and plutonium.

Description

Diluent and preparation and application thereof
Technical Field
The invention relates to a preparation method of a diluent, in particular to a preparation method of a diluent required in a Purex process.
Background
The spent fuel post-processing technology is the most critical link in the later stage of nuclear fuel cycle and is one of the key technologies for guaranteeing the sustainable development of nuclear energy. Spent fuel reprocessing is the chemical separation of uranium and plutonium from fission products from uranium wastes that have been used at 3% to 4%. The recovered uranium and plutonium are recycled in the mixed oxide fuel of the nuclear power plant to produce more energy, so that uranium resources are more fully utilized and the demand for uranium enrichment is reduced.
The Purex process is the most successful and widely applied process in the international spent fuel post-treatment at present, tributyl phosphate (TBP) is contacted with a spent fuel nitric acid aqueous solution, the TBP selectively extracts uranium and plutonium, and the extraction rate of cracking products and impurities thereof is extremely low. Uranium and plutonium are then separated from the fission products by multistage countercurrent extraction. TBP has the advantages of good chemical stability, high flash point, low volatility, poor miscibility with water, easy regeneration and the like, and is the most suitable extractant at present. However, TBP has a high density and viscosity, and is not easily contacted with uranium or plutonium in an aqueous phase, and it needs to be diluted in order to obtain an optimum extraction effect. Currently, the common diluents are n-dodecane and higher kerosene. However, there is still room for improvement in the extraction performance of the existing TBP + n-dodecane/higher kerosene. Therefore, in order to improve the extraction efficiency of uranium and plutonium from spent fuel, the development of diluents with higher performance is still needed.
Disclosure of Invention
The invention aims to provide a preparation method of a novel diluent with better performance than n-dodecane and high kerosene.
Based on the purpose, the invention adopts the technical scheme that:
a) Taking Fischer-Tropsch distillate as a raw material and Pt/SAPO-11@ beta as a catalyst, and reacting at a reaction pressureThe force is 1.0MPa to 7.0MPa, preferably 1.0MPa to 4.0MPa, the reaction temperature is 100 ℃ to 500 ℃, preferably 250 ℃ to 400 ℃, and the space velocity is 0.5h -1 -7h -1 Preferably 0.5h -1 -3h -1 The hydrogen-oil ratio is 200;
b) And (4) rectifying and separating out middle distillate from the obtained isoparaffin to obtain the target diluent.
The Fischer-Tropsch distillate oil in the step A) comprises 75% of C11-C12 alkane, less than 5% of C5-C9 fraction, less than 5% of C14-C17 fraction and the balance of C10 and C13 in percentage by mass. The C12 alkane in the C11-C12 alkane contains more than 40% of C10-C12 alkane raw material by mass.
4. The method of claim 1, wherein: the mass fraction of Pt in the catalyst Pt/SAPO-11@ beta is 0.1-3 wt%, preferably 0.5-2 wt%, the Si/Al ratio of the beta molecular sieve is 20-40, and the mass ratio of SAPO-11 to the beta molecular sieve is 50.
During the rectification treatment in the step B), the theoretical plate number of the rectification tower is 100-200 (preferably 150-200), and the temperature of the kettle in the rectification tower is as follows: 80-140 ℃ (preferably 90-120 ℃), and the kettle pressure is as follows: 0.1kPa to 1kPa (preferably 0.2kPa to 0.6 kPa), and fractions with overhead vapor temperatures of 50 ℃ to 75 ℃ (preferably 55 ℃ to 70 ℃) are collected at a reflux ratio of: 10-20 (preferably 10-15).
The novel diluent prepared by the method is used for a spent fuel extracting agent, and can selectively extract and separate uranium and plutonium when the novel diluent is contacted with a nitric acid aqueous solution with the molar concentration of spent fuel of 3.0mol/L-4.0 mol/L.
The invention provides a preparation method of a high-performance diluent, aiming at the problem of low extraction performance of the existing diluent.
Detailed Description
To further illustrate the present invention, the following examples are set forth without limiting the scope of the invention as defined by the various appended claims.
Example 1
Preparation of the catalyst:
preparing a precursor Pt (NH) of Pt according to the mass percent of 0.5 percent 3 ) 4 Cl 2 Grinding and uniformly mixing SAPO-11 and beta molecular sieve with the mass ratio of 20 to 1 in an aqueous solution (the mass concentration of Pt is 1 mg/ml), tabletting and forming, crushing and screening out particles of 20 to 40 meshes, and placing the SAPO-11@ beta molecular sieve of 20 to 40 meshes in Pt (NH) 3 ) 4 Cl 2 And standing the solution for 24 hours, separating out solids, drying the solids in an oven at the temperature of 110 ℃ overnight, and then roasting the solids at the temperature of 550 ℃ for 6 hours to obtain the Pt/SAPO-11@ beta catalyst.
Raw material isomerization reaction:
before reaction, pt/SAPO-11@ beta catalyst is in H at 20ml/min 2 Reducing for 2h at 400 ℃ under the atmosphere, taking Fischer-Tropsch distillate as a raw material, and reacting at the reaction temperature: 350 ℃ and reaction pressure: 2MPa, space velocity: 1h -1 Hydrogen-oil ratio: carrying out hydroisomerization reaction under the reaction condition of 1200.
And (3) rectification of an isomerization product:
the theoretical plate number of the rectifying tower is 200, and the temperature of the kettle in the rectifying tower is as follows: 100-125 ℃ and the kettle pressure is as follows: 0.5kPa, collecting the fraction with the overhead vapor temperature of 55-68 ℃, and the reflux ratio is as follows: the isomerization product alkane is rectified under the rectification condition of 10, and the cut product is the target diluent (according to the mass percentage content, the content of C10-C12 isoparaffin is 95.6 percent, wherein the content of C12 is 54 percent of the mass of the diluent, the content of C8 below is 0.4 percent, the content of C14 above is 0.7 percent, and the rest is C9 and C13 fractions).
Extraction test of diluent:
1. phase separation time: preparing into TBP-diluent solution at 30% by volume, and mixing with 1mol/L HNO 3 Or the equal-volume oscillation of 1mol/L NaOH solution, fully mixing, standing and recording the phase separation time, wherein the phase separation time of the two systems is the same and is 1min.
Mixing the volume ratio of the mixture to 30% of TBP-n-dodecane solution with 1mol/L of HNO 3 Oscillating the solution in equal volume, fully mixing, standing and recording the phase separation time, wherein the phase separation time of the two systems is the same and is 1.5min; the phase separation time of the target diluent is 1min better than 1.5min of n-dodecane.
2. And (3) testing extraction performance: preparing into TBP-diluent solution 30 vol%, and mixing with HNO 3.5mol/L 3 The dissolved molar concentration of 0.55mol/LPu (IV) metal ion solution was mixed well at a volume ratio of 1:1 and the saturated extraction capacity of metal in 30% TBP-diluent solution was determined. The TBP-target diluent extraction saturation capacity was 80g/L as determined by 30% and the TBP-n-dodecane extraction saturation capacity was 58g/L as determined by 30%.
Example 2
The target diluent obtained in the same manner as described in example 1 except that the reaction temperature in the raw material hydrogenation step was changed to 280 ℃ was subjected to the extraction test (using 1mol/L HNO) under the conditions of example 1 3 Determination of phase separation time) 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity 60g/L.
Example 3
The target diluent obtained in the same manner as described in example 1 except that the reaction temperature in the raw material hydrogenation step was changed to 300 ℃ was subjected to the extraction test (using 1mol/L HNO) under the conditions of example 1 3 Determination of phase separation time) 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity 65g/L.
Example 4
The target diluent obtained in the same manner as described in example 1 except that the reaction temperature in the raw material hydrogenation step was changed to 325 deg.C was subjected to the extraction test (using 1mol/L HNO) under the conditions of example 1 3 Determination of phase separation time) 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity 72g/L.
Example 5
The target diluent obtained in the same manner as described in example 1 except that the reaction temperature in the raw material hydrogenation step was changed to 375 deg.C was used, and the extraction experiment test (using 1mol/L HNO) was carried out under the same conditions as in example 1 3 Measurement of phase separation time) in the extraction test process, the phase separation time is 1min better than dodecane, 30The% TBP-target diluent extraction saturation capacity was 79g/L.
Example 6
The objective diluent obtained in the same manner as described in example 1 except that the reaction temperature in the raw material hydrogenation reaction step was changed to 400 deg.C, and the extraction experimental test was carried out under the same conditions as in example 1 (using 1mol/L of HNO) 3 Determination of phase separation time) 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity was 76g/L.
Example 7
The target diluent obtained in the same manner as described in example 1 except that the reaction pressure in the raw material hydrogenation step was changed to 1MPa, and the extraction experiment test (using 1mol/L HNO) was carried out under the conditions of example 1 3 Determination of phase separation time) was better than dodecane for 1min during the extraction test, 30% TBP-the target diluent extraction saturation capacity was 70g/L.
Example 8
The target diluent obtained in the same manner as described in example 1 except that the reaction pressure in the raw material hydrogenation step was changed to 3MPa, and the extraction experiment test (using 1mol/L HNO) was carried out under the conditions of example 1 3 Determination of phase separation time) 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity was 78g/L.
Example 9
The target diluent obtained in the same manner as described in example 1 except that the reaction pressure in the raw material hydrogenation step was changed to 4MPa, and the extraction experiment test (using 1mol/L HNO) was carried out under the conditions of example 1 3 Determination of phase separation time) 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity 82g/L.
Example 10
Except that the hollow speed in the step of the hydrogenation reaction of the raw material is changed into 0.5h -1 In addition, the target diluent obtained in the same manner as described in example 1 was subjected to an extraction test (using 1mol/L of HNO) under the conditions of example 1 3 Determination of phase separation time) 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity 85g/L.
Example 11
Except that the hollow speed in the step of the hydrogenation reaction of the raw material is changed into 1.5h -1 In addition, the target diluent obtained in the same manner as described in example 1 was subjected to an extraction test (using 1mol/L of HNO) under the conditions of example 1 3 Determination of phase separation time) 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity was 78g/L.
Example 12
Except that the hollow speed in the step of the raw material hydrogenation reaction is changed into 2h -1 In addition, the target diluent obtained in the same manner as described in example 1 was subjected to an extraction test (using 1mol/L of HNO) under the conditions of example 1 3 Determination of phase separation time) 1min was better than dodecane during the extraction test 30% tbp-target diluent extraction saturation capacity of 73g/L.
Example 13
Except that the hollow speed in the step of hydrogenation reaction of raw materials is changed into 2.5h -1 In addition, the target diluent obtained in the same manner as described in example 1 was subjected to an extraction test (using 1mol/L of HNO) under the conditions of example 1 3 Determination of phase separation time) 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity 71g/L.
Example 14
Except that the hollow speed is changed to 3h in the step of hydrogenation reaction of raw materials -1 In addition, the target diluent obtained in the same manner as described in example 1 was subjected to an extraction test (using 1mol/L of HNO) under the conditions of example 1 3 Determination of phase separation time) 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity 65g/L.
Example 15
Except that the hydrogen-to-oil ratio in the feed hydrogenation step was changed to 600:1, in the same phase as described in example 1The target diluent obtained in the same manner was subjected to extraction test (using 1mol/L HNO) under the conditions of example 1 3 Measured phase separation time) was determined, the phase separation time was 1min better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity was 72g/L.
Example 16
Except that the hydrogen-oil ratio in the step of hydrogenation reaction of raw materials is changed to 800:1 in addition, the target diluent obtained in the same manner as described in example 1 was subjected to the extraction test (using 1mol/L HNO) under the conditions of example 1 3 Determination of phase separation time) during the extraction test, a phase separation time of 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity of 78g/L.
Example 17
Except that the hydrogen-oil ratio in the step of hydrogenation reaction of the raw material was changed to 1000:1 in addition, the target diluent obtained in the same manner as described in example 1 was subjected to the extraction test (using 1mol/L HNO) under the conditions of example 1 3 Determination of phase separation time) during the extraction test, a phase separation time of 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity of 82g/L.
Example 18
Except that the hydrogen-to-oil ratio in the feed hydrogenation step was changed to 1500:1 in addition, the target diluent obtained in the same manner as described in example 1 was subjected to the extraction test (using 1mol/L HNO) under the conditions of example 1 3 Determination of phase separation time) during the extraction test, a phase separation time of 1min was better than dodecane during the extraction test, 30% tbp-target diluent extraction saturation capacity of 80g/L.

Claims (6)

1. Use of a diluent, characterized in that: the extraction agent is used for the spent fuel, and can selectively extract and separate uranium and plutonium when being contacted with a nitric acid aqueous solution with the molar concentration of the spent fuel of 3.0mol/L-4.0 mol/L;
the preparation method of the diluent comprises the following steps:
a) From Fischer-Tropsch distillates andhydrogen is used as raw material, pt/SAPO-11@ beta is used as catalyst, the reaction pressure is 1.0MPa-7.0MPa, the reaction temperature is 100-500 ℃, and the airspeed is 0.5h -1 ～7 h -1 The hydrogen-oil ratio is 200;
b) Rectifying the obtained isoparaffin fraction to obtain a target diluent; during rectification treatment, the theoretical plate number of the rectification tower is 100-200, and the temperature of the kettle in the rectification tower is as follows: the temperature is 80-140 ℃, and the kettle pressure is as follows: 0.1kPa to 1kPa, collecting fractions with the overhead vapor temperature of 50 ℃ to 75 ℃ as target diluents, and the reflux ratio is as follows: 10 to 20;
the Fischer-Tropsch distillate comprises, by mass percentage, over 75% of C11-C12 alkane fraction, less than 5% of C5-C9 alkane fraction, less than 5% of C14-C17 alkane fraction and the balance of C10 and/or C13 alkane fraction.
2. Use according to claim 1, characterized in that: the mass content of C12 alkanes in the C11-C12 alkane fraction is > 40%.
3. Use according to claim 1, characterized in that: the mass fraction of Pt in the catalyst Pt/SAPO-11@ beta is 0.1-3 wt%, the Si/Al ratio of the beta molecular sieve is 20-40, and the mass ratio of the SAPO-11 to the beta molecular sieve is 50.
4. Use according to claim 1, characterized in that: the concentration of metal ions uranium and plutonium in the spent fuel is 0.4-0.7 mol/L.
5. Use according to claim 1, characterized in that: in the step A), the reaction pressure is 1.0-4.0MPa, the reaction temperature is 250-400 ℃, and the space velocity is 0.5h -1 -3 h -1 The hydrogen-oil ratio is 600;
the mass fraction of Pt in the catalyst Pt/SAPO-11@ beta is 0.5-2 wt%, and the mass ratio of the SAPO-11 to the beta molecular sieve is (40).
6. Use according to claim 1, characterized in that: during rectification treatment, the theoretical plate number of a rectification tower is 150-200, the temperature of a kettle in the rectification tower is 90-120 ℃, and the kettle pressure is as follows: 0.2kPa-0.6kPa, collecting fraction with the tower top steam temperature of 55-70 ℃ as a target diluent, wherein the reflux ratio is as follows: 10 to 15.
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CN104560193A (en) * 2013-10-28 2015-04-29 中国石油化工股份有限公司 Preparation method of base oil and/or solvent oil of lubricating oil
CN105132017A (en) * 2015-09-08 2015-12-09 天津大学 Preparation method of coal-based jet fuel

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Title
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