CN101575089A - Method for preparing <18>O-nitric acid - Google Patents
Method for preparing <18>O-nitric acid Download PDFInfo
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- CN101575089A CN101575089A CNA2009100528543A CN200910052854A CN101575089A CN 101575089 A CN101575089 A CN 101575089A CN A2009100528543 A CNA2009100528543 A CN A2009100528543A CN 200910052854 A CN200910052854 A CN 200910052854A CN 101575089 A CN101575089 A CN 101575089A
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Abstract
The invention relates to a method for preparing <18>O-nitric acid, comprising the following steps of: (1) carrying out oxygen isotope exchange reaction between nitric acid material and oxygen-18 water in a sealed reaction kettle at the temperature between 50 DEG C and 80 DEG C for 1 to 10 days; (2) introducing ammonia gas to solution obtained after reaction for neutralization and removing oxygen-18 water with reduced abundance ratio through distillation at reduced pressure to obtain <18>O-ammonium nitrate crystals in the reaction kettle; and (3) adding excessive acid to the reaction kettle to fully dissolve the <18>O-ammonium nitrate crystals in the reaction kettle so as to regenerate <18>O-nitric acid, and carrying out distillation at reduced pressure again to distill the regenerated <18>O-nitric acid into liquid nitrogen trap so as to obtain the <18>O-nitric acid product. Compared with the prior art, the invention has the advantages of simple process, easy operation, low energy consumption, high purity of products and low loss of <18>O and the like.
Description
Technical field
The present invention relates to a kind of preparation method of stable isotope oxygen-18 tagged compound, especially relate to a kind of
18The preparation method of O-nitric acid.
Background technology
Occurring in nature oxygen (O) unit have three kinds of stable isotopes:
16O,
17O,
18O, total mass number is respectively 16,17,18, and natural abundance is respectively 99.76%, 0.036%, 0.204%, and all "dead", all is stable isotope.Oxygen-18 is as a kind of stable isotope, its application mainly is a character of utilizing isotropic substance physics close with chemical property, i.e. " isotopic tracer technique ", as be applied to the research of organism metabolism, the control of medicine synthesis step, environmental science and water geology, chemical chain characteristic and aspects such as chemical reaction mechanism, nuclear medicine diagnostic.
According to different needs, oxygen-18 isotropic substance can synthesize different tagged compounds.For example by hydrogen and oxygen-18 isotropic substance bonded product weigh oxygen (
18O) water is also referred to as oxygen-18 water, and molecular formula is H
2 18O, molecular weight are 20.0, its chemical property and ortho-water (H
2 16O) identical, heavy oxygen (
18O) water is widely used in the nuclear medicine diagnostic technical field as nuclear medicine diagnosis reagent, and especially the fast development of nuclear medicine image technology PET (Positron Emission Computed Tomography technology) causes heightening as the heavy oxygen water of nuclear medicine diagnosis reagent consumption.
Nitric acid (HNO
3) be a kind of important chemical material, the acid that in industrial and laboratory, all is in daily use.As the essential raw material of nitrate and nitric ether, nitric acid is used to produce a series of Nitrates nitrogenous fertilizer, as ammonium nitrate, saltpetre etc., nitric acid and ammonia effect generate ammonium nitrate, it also is a kind of chemical fertilizer, and nitrogen content all has higher fertilizer efficiency than ammonium sulfate height for various soil.With oxygen-18 isotopic labeling extremely
18O-nitric acid (HN
18O
3), can make multiple tagged compound, especially make chemical fertilizer such as ammonium nitrate, saltpetre, particularly the metabolism research of farm crop and phytosynthesis carbohydrate and proteinic mechanism are significant for the research plant.
Summary of the invention
Purpose of the present invention be exactly provide in order to overcome the defective that prior art exists that a kind of technology is simple, easy to operate, less energy consumption, product purity height,
18The O loss is few
18The preparation method of O-nitric acid.
Purpose of the present invention can be achieved through the following technical solutions: a kind of
18The preparation method of O-nitric acid is characterized in that, this preparation method specifically may further comprise the steps:
(1) nitric acid material and oxygen-18 water are carried out the permutoid reaction of oxygen isotope in reactor, temperature is controlled at 50～80 ℃, and the entire reaction still keeps air-tight state, and the reaction times was controlled at 1～10 day, and the mole proportioning of nitric acid and oxygen-18 water was at 1: 3～1: 20;
(2) feed the ammonia neutralization in reacted solution, oxygen-18 water that abundance has reduced is removed in underpressure distillation, and pressure-controlling is at 50～200mmHg, and temperature is controlled at 40～70 ℃, obtains in reactor
18The O-ammonium nitrate crystal;
(3) in reactor, add excessive acid, in the abundant solubilizing reaction still
18The O-ammonium nitrate crystal regenerates
18O-nitric acid carries out underpressure distillation again, and pressure-controlling is at 50～200mmHg, and temperature is controlled at 40～70 ℃, with what generate
18O-nitric acid steams in the liquid nitrogen cold trap, thereby obtains
18O-nitric acid product.
Described nitric acid material
18The atomic percent of O is 0.2%～98%.
Described nitric acid material is
18O is natural abundance or reacted through Oxygen isotope exchange
18O-nitric acid product.
Described oxygen-18 water
18The atomic percent of O＞98%.
Acid in the described step (3) is selected from a kind of in sulfuric acid, hydrochloric acid, trifluoroacetic acid, methylsulfonic acid, the phenylformic acid.
Described
18O-nitric acid product and oxygen-18 water repeat above-mentioned steps (1)-(3), obtain abundant
18O-nitric acid product.
Described
18O-nitric acid product
18The atomic percent of O is 10%～98%.
Compared with prior art, the present invention carries out isotope exchange reaction with the nitric acid and oxygen-18 water of natural abundance in reactor, finally can obtain abundant
18O-nitric acid product.Technology of the present invention is simple, easy to operate, less energy consumption, product purity height,
18The O loss is few.
Description of drawings
Fig. 1 is preparation
18The device synoptic diagram of O-nitric acid.
Among the figure: 1-thermostatically heating still, 2-reactor, 3-thermometer, 4-vacuum buffer pipe, 5-cold-trap, 6-liquid nitrogen cold trap.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
Be preparation as shown in Figure 1
18The device synoptic diagram of O-nitric acid.Earlier with a certain amount of oxygen-18 water (
18O abundance＞98%) put into reactor 2, slowly add a certain amount of nitric acid again, reactor 2 is a there-necked flask, wherein middle port is provided with the temperature that thermometer 3 is measured reactor 2, left side mouth is provided with vacuum buffer pipe 4, and the right mouth is provided with cold-trap 5, and cold-trap 5 connects liquid nitrogen cold trap 6.By thermostatically heating still 1 temperature is controlled at 50～80 ℃ and keep the air-tight state of entire reaction still 2, allow nitric acid and oxygen-18 water in reactor 2, carry out the permutoid reaction of oxygen isotope with this understanding, reaction times was controlled at 1～10 day, the mole proportioning of nitric acid and oxygen-18 water was at 1: 3～1: 20, and reaction times and mole proportioning can be according in the nitric acid
18The O abundance is adjusted, if in the nitric acid
18The O abundance is higher can be reduced the reaction times and reduce nitric acid and the mole proportioning of oxygen-18 water.In order to follow the tracks of the process of permutoid reaction, the sample that can take a morsel in reaction process changes into nitric acid with acid again with ammonia neutralization, evaporation, adds the dichloromethane solution of methyl-phenoxide, utilize mass spectroscopy 4-(nitro-
18O
2) methyl-phenoxide, promptly as can be known in the nitric acid
18The abundance of O.Feed the excessive ammonia neutralization in the reacted solution, underpressure distillation removes deoxidation-18 water, and pressure-controlling is at 50～200mmHg, and temperature is controlled at 40～70 ℃, obtains white in reactor
18The O-ammonium nitrate crystal.In reactor, add excessive acid again, in the abundant solubilizing reaction still
18The O-ammonium nitrate crystal regenerates
18O-nitric acid carries out underpressure distillation again, and pressure-controlling is at 50～200mmHg, and temperature is controlled at 40～70 ℃, with what generate
18O-nitric acid steams in the liquid nitrogen cold trap, can obtain in liquid nitrogen cold trap
18O-nitric acid product.To obtain
18O-nitric acid product can with oxygen-18 water (
18O abundance＞98%) repeats above process, thereby obtain abundant
18O-nitric acid product.
Reaction equation of the present invention is:
HNO
3+H
2 18O＝HN
18O
3+H
2O
HN
18O
3+NH
3＝NH
4N
18O
3
NH
4N
18O
3+H*R＝HN
18O
3+NH
4*R
Will
18The O abundance be 0.2% nitric acid 2mol and oxygen-18 water 25mol (
18The O abundance is 98.5%) in reactor, carry out the permutoid reaction of oxygen isotope, temperature is controlled at 70 ℃, and the entire reaction still keeps air-tight state, and the reaction times is 10 days.Feed the neutralization of excess of ammonia gas in reacted solution, underpressure distillation removes deoxidation-18 water, and pressure-controlling is at 80mmHg, and temperature is controlled at 40～42 ℃, obtains in reactor
18The O-ammonium nitrate crystal.In reactor, add excessive methylsulfonic acid, in the abundant solubilizing reaction still
18The O-ammonium nitrate crystal regenerates
18O-nitric acid carries out underpressure distillation again, and pressure-controlling is at 80mmHg, and temperature is controlled at 40～42 ℃, with what generate
18O-nitric acid steams in the liquid nitrogen cold trap, thereby obtains
18The O abundance is 16%
18O-nitric acid product 0.8mol.
Embodiment 2
Will
18The O abundance be 39% nitric acid 1.2mol and oxygen-18 water 10mol (
18The O abundance is 98.5%) in reactor, carry out the permutoid reaction of oxygen isotope, temperature is controlled at 70 ℃, and the entire reaction still keeps air-tight state, and the reaction times is 6 days.Feed the neutralization of excess of ammonia gas in reacted solution, underpressure distillation removes deoxidation-18 water, and pressure-controlling is at 100mmHg, and temperature is controlled at 48～52 ℃, obtains in reactor
18The O-ammonium nitrate crystal.In reactor, add excessive hydrochloric acid, in the abundant solubilizing reaction still
18The O-ammonium nitrate crystal regenerates
18O-nitric acid carries out underpressure distillation again, and pressure-controlling is at 100mmHg, and temperature is controlled at 48～52 ℃, with what generate
18O-nitric acid steams in the liquid nitrogen cold trap, thereby obtains
18The O abundance is 76%
18O-nitric acid product 0.6mol.
A kind of
18The preparation method of O-nitric acid, this preparation method specifically may further comprise the steps:
(1) will be through after the isotope exchange reaction
18The O-nitric acid material with
18The oxygen of O abundance＞98%-18 water carries out the permutoid reaction of oxygen isotope in reactor, described
18The O-nitric acid material
18The atomic percent of O abundance is 98%, and temperature is controlled at 50 ℃, and the entire reaction still keeps air-tight state, and the reaction times was controlled at 10 days, and the mole proportioning of nitric acid and oxygen-18 water was at 1: 20;
(2) feed the ammonia neutralization in reacted solution, oxygen-18 water that abundance has reduced is removed in underpressure distillation, and pressure-controlling is at 50mmHg, and temperature is controlled at 70 ℃, obtains in reactor
18The O-ammonium nitrate crystal;
(3) in reactor, add excessive trifluoroacetic acid, in the abundant solubilizing reaction still
18The O-ammonium nitrate crystal regenerates
18O-nitric acid carries out underpressure distillation again, and pressure-controlling is at 50mmHg, and temperature is controlled at 70 ℃, with what generate
18O-nitric acid steams in the liquid nitrogen cold trap, thereby obtains
18O-nitric acid product obtains
18O-nitric acid product
18The atomic percent of O is 20%.
A kind of
18The preparation method of O-nitric acid, this preparation method specifically may further comprise the steps:
(1) with natural abundance
18The O-nitric acid material with
18The O abundance is 99% oxygen-18 water carries out oxygen isotope in reactor permutoid reaction, and is described
18The O-nitric acid material
18The atomic percent of O abundance is 0.2%, and temperature is controlled at 80 ℃, and the entire reaction still keeps air-tight state, and the reaction times was controlled at 1 day, and the mole proportioning of nitric acid and oxygen-18 water was at 1: 3;
(2) feed the ammonia neutralization in reacted solution, oxygen-18 water that abundance has reduced is removed in underpressure distillation, and pressure-controlling is at 200mmHg, and temperature is controlled at 40 ℃, obtains in reactor
18The O-ammonium nitrate crystal;
(3) in reactor, add excessive sulfuric acid, in the abundant solubilizing reaction still
18The O-ammonium nitrate crystal regenerates
18O-nitric acid carries out underpressure distillation again, and pressure-controlling is at 200mmHg, and temperature is controlled at 40 ℃, with what generate
18O-nitric acid steams in the liquid nitrogen cold trap, thereby obtains
18O-nitric acid product obtains
18O-nitric acid product
18The atomic percent of O is 10%.
Embodiment 5
A kind of
18The preparation method of O-nitric acid, this preparation method specifically may further comprise the steps:
(1) with natural abundance
18The O-nitric acid material with
18The O abundance is 99.99% oxygen-18 water carries out oxygen isotope in reactor permutoid reaction, and is described
18The O-nitric acid material
18The atomic percent of O abundance is 10%, and temperature is controlled at 60 ℃, and the entire reaction still keeps air-tight state, and the reaction times was controlled at 3 days, and the mole proportioning of nitric acid and oxygen-18 water was at 1: 10;
(2) feed the ammonia neutralization in reacted solution, oxygen-18 water that abundance has reduced is removed in underpressure distillation, and pressure-controlling is at 100mmHg, and temperature is controlled at 50 ℃, obtains in reactor
18The O-ammonium nitrate crystal;
(3) in reactor, add excessive sulfuric acid, in the abundant solubilizing reaction still
18The O-ammonium nitrate crystal regenerates
18O-nitric acid carries out underpressure distillation again, and pressure-controlling is at 100mmHg, and temperature is controlled at 60 ℃, with what generate
18O-nitric acid steams in the liquid nitrogen cold trap, thereby obtains
18O-nitric acid product.
With what obtain
18O-nitric acid product and oxygen-18 water repeat above-mentioned steps (1)-(3), obtain abundant
18O-nitric acid product should
18O-nitric acid product
18The atomic percent of O is 98%.
A kind of
18The preparation method of O-nitric acid, this preparation method specifically may further comprise the steps:
(1) with natural abundance
18O-nitric acid product with
18The O abundance is 99.98% oxygen-18 water carries out oxygen isotope in reactor permutoid reaction, and is described
18O-nitric acid product
18The atomic percent of O abundance is 50%, and temperature is controlled at 65 ℃, and the entire reaction still keeps air-tight state, and the reaction times was controlled at 5 days, and the mole proportioning of nitric acid and oxygen-18 water was at 1: 15;
(2) feed the ammonia neutralization in reacted solution, oxygen-18 water that abundance has reduced is removed in underpressure distillation, and pressure-controlling is at 150mmHg, and temperature is controlled at 65 ℃, obtains in reactor
18The O-ammonium nitrate crystal;
(3) in reactor, add excessive sulfuric acid, in the abundant solubilizing reaction still
18The O-ammonium nitrate crystal regenerates
18O-nitric acid carries out underpressure distillation again, and pressure-controlling is at 150mmHg, and temperature is controlled at 65 ℃, with what generate
18O-nitric acid steams in the liquid nitrogen cold trap, thereby obtains
18O-nitric acid product obtains
8O-nitric acid product
18The atomic percent of O is 80%.
Claims (7)
1. one kind
18The preparation method of O-nitric acid is characterized in that, this preparation method specifically may further comprise the steps:
(1) nitric acid material and oxygen-18 water are carried out the permutoid reaction of oxygen isotope in reactor, temperature is controlled at 50～80 ℃, and the entire reaction still keeps air-tight state, and the reaction times was controlled at 1～10 day, and the mole proportioning of nitric acid and oxygen-18 water was at 1: 3～1: 20;
(2) feed the ammonia neutralization in reacted solution, oxygen-18 water that abundance has reduced is removed in underpressure distillation, and pressure-controlling is at 50～200mmHg, and temperature is controlled at 40～70 ℃, obtains in reactor
18The O-ammonium nitrate crystal;
(3) in reactor, add excessive acid, in the abundant solubilizing reaction still
18The O-ammonium nitrate crystal regenerates
18O-nitric acid carries out underpressure distillation again, and pressure-controlling is at 50～200mmHg, and temperature is controlled at 40～70 ℃, with what generate
18O-nitric acid steams in the liquid nitrogen cold trap, thereby obtains
18O-nitric acid product.
2. according to claim 1 a kind of
18The preparation method of O-nitric acid is characterized in that, described nitric acid material
18The atomic percent of O is 0.2%～98%.
3. according to claim 1 and 2 a kind of
18The preparation method of O-nitric acid is characterized in that, described nitric acid material is
18O is natural abundance or reacted through Oxygen isotope exchange
18O-nitric acid product.
4. according to claim 1 a kind of
18The preparation method of O-nitric acid is characterized in that, described oxygen-18 water
18The atomic percent of O＞98%.
5. according to claim 1 a kind of
18The preparation method of O-nitric acid is characterized in that, the acid in the described step (3) is selected from a kind of in sulfuric acid, hydrochloric acid, trifluoroacetic acid, methylsulfonic acid, the phenylformic acid.
6. according to claim 1 a kind of
18The preparation method of O-nitric acid is characterized in that, and is described
18O-nitric acid product and oxygen-18 water repeat above-mentioned steps (1)-(3), obtain abundant
18O-nitric acid product.
7. according to claim 1 a kind of
18The preparation method of O-nitric acid is characterized in that, and is described
18O-nitric acid product
18The atomic percent of O is 10%～98%.
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|---|---|---|---|
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| CN101575089B CN101575089B (en) | 2010-12-29 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111268678A (en) * | 2020-03-12 | 2020-06-12 | 江苏华益科技有限公司 | Preparation method, device and application of high-abundance oxygen-18 carbon dioxide |
| CN113735077A (en) * | 2020-05-29 | 2021-12-03 | 中国科学院沈阳应用生态研究所 | Preparation method15N and18o double labeling of N2Method of O |
| CN115025727A (en) * | 2021-10-23 | 2022-09-09 | 苏州思萃同位素技术研究所有限公司 | Preparation device and preparation method of oxygen isotope oxalic acid |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1113878A (en) * | 1994-06-01 | 1995-12-27 | 门伟 | Producing method for sulfuric acid, nitric acid and hydrochloric acid |
| US6165435A (en) * | 1998-12-24 | 2000-12-26 | Praxair Technology, Inc. | Method and production of nitric acid |
-
2009
- 2009-06-10 CN CN2009100528543A patent/CN101575089B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111268678A (en) * | 2020-03-12 | 2020-06-12 | 江苏华益科技有限公司 | Preparation method, device and application of high-abundance oxygen-18 carbon dioxide |
| CN113735077A (en) * | 2020-05-29 | 2021-12-03 | 中国科学院沈阳应用生态研究所 | Preparation method15N and18o double labeling of N2Method of O |
| CN113735077B (en) * | 2020-05-29 | 2023-07-07 | 中国科学院沈阳应用生态研究所 | Preparation method 15 N and 18 o double-labeled N 2 O method |
| CN115025727A (en) * | 2021-10-23 | 2022-09-09 | 苏州思萃同位素技术研究所有限公司 | Preparation device and preparation method of oxygen isotope oxalic acid |
| CN115025727B (en) * | 2021-10-23 | 2024-04-30 | 苏州思萃同位素技术研究所有限公司 | Preparation device and preparation method of oxygen isotope oxalic acid |
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| CN101575089B (en) | 2010-12-29 |
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Assignee: Anhui Jinhe Stock Co., Ltd. Assignor: Shanghai Chemical Research Institute|Shanghai union Isotope Technology Co., Ltd. Contract record no.: 2011340000533 Denomination of invention: Method for preparing [sup]18[/sup]O- nitric acid Granted publication date: 20101229 License type: Exclusive License Open date: 20091111 Record date: 20111230 |
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Address after: 200062 Shanghai city Putuo District Yunling Road No. 345 Co-patentee after: Shanghai Lianhong Isotope Technology Co., Ltd. Patentee after: Shanghai Chemical Research Institute Co., Ltd. Address before: 200062 Shanghai city Putuo District Yunling Road No. 345 Co-patentee before: Shanghai Lianhong Isotope Technology Co., Ltd. Patentee before: Shanghai Research Institute of Chemical Industry |