阅读说明：本技术 一种含柠嗪酸阴离子的离子液体及其在碘吸收中的应用 (Ionic liquid containing citrazinic acid anions and application thereof in iodine absorption ) 是由 陈钰 王树军 梁红莲 于 2020-04-28 设计创作，主要内容包括：本申请公开了一种含柠嗪酸阴离子的离子液体在碘吸收中的应用,包括以下步骤：1)将柠嗪酸和碱性物质按摩尔比在一定条件下搅拌混合,得到混合物一；2)将步骤1)制备的混合物一进行干燥,得到柠嗪酸型离子液体；3)将步骤2)制备的柠嗪酸型离子液体在一定条件下吸收碘；4)取步骤3)制备的离子液体和碘的混合物,检测离子液体中碘的吸收容量。本发明的优点在于它能克服现有技术的弊端,方法简单,易于操作,条件温和,原料便宜,且对环境友好。(The application discloses an application of ionic liquid containing citrazinic acid anions in iodine absorption, which comprises the following steps: 1) stirring and mixing citrazinic acid and an alkaline substance according to a certain molar ratio under a certain condition to obtain a first mixture; 2) drying the mixture I prepared in the step 1) to obtain citrazinic acid type ionic liquid; 3) absorbing iodine by the citrazinic acid type ionic liquid prepared in the step 2) under a certain condition; 4) taking the mixture of the ionic liquid and iodine prepared in the step 3), and detecting the absorption capacity of iodine in the ionic liquid. The invention has the advantages that the invention can overcome the defects of the prior art, and has simple method, easy operation, mild condition, cheap raw materials and environmental protection.)

1. The ionic liquid containing the citrazinic acid anion is characterized in that: the ionic liquid has a chemical structural formula as shown in formula (1) or (2):

2. the ionic liquid containing citrazinic acid anions according to claim 1, wherein: the ionic liquid of formula (1) is prepared by mixing citrazinic acid with tetrabutylammonium hydroxide, and the ionic liquid of formula (2) is prepared by mixing citrazinic acid with tetrabutylphosphorus hydroxide.

3. Use of ionic liquids containing citrazinate anions according to claims 1 to 2 for iodine absorption, characterized in that: the method comprises the following steps:

1) stirring and mixing citrazinic acid and an alkaline substance according to a certain molar ratio under a certain condition to obtain a first mixture;

2) drying the mixture I prepared in the step 1) to obtain citrazinic acid type ionic liquid;

3) absorbing iodine by the citrazinic acid type ionic liquid prepared in the step 2) under a certain condition;

4) taking the mixture of the ionic liquid and iodine prepared in the step 3), and detecting the absorption capacity of iodine in the ionic liquid.

4. The use of ionic liquids containing citrazinic acid anions according to claim 3, characterized in that: in the step 1), the molar ratio of the citrazinic acid to the basic substance contained in the first mixture is 1:1 to 1: 3.

5. The use of ionic liquids containing citrazinic acid anions according to claim 3, characterized in that: in step 1), the alkaline substance can be one or more of a mixture of tetrabutyl phosphorus hydroxide aqueous solution, tetrabutyl ammonium hydroxide aqueous solution and tetraethyl ammonium hydroxide aqueous solution; the mass fraction of the alkaline substance in the aqueous solution is 10 to 40 percent.

6. The use of ionic liquids containing citrazinic acid anions according to claim 3, characterized in that: in the step 1), when the citrazinic acid and the alkaline substance are stirred and mixed according to the molar ratio, the mixing temperature is kept between 30 and 90 ℃, and the stirring and mixing time is 10 hours.

7. The use of ionic liquids containing citrazinic acid anions according to claim 3, characterized in that: in step 2), when the mixture prepared in step 1) is dried, the drying method may be one or more of vacuum oven drying, rotary evaporation drying and freeze drying.

8. The use of ionic liquids containing citrazinic acid anions according to claim 3, characterized in that: in the step 3), when the citrazinic acid type ionic liquid absorbs iodine under a certain condition, the absorption condition can be that iodine is prepared into iodine vapor or iodine is prepared into a cyclohexane iodine solution; in step 4), when the absorption capacity of iodine in the ionic liquid is detected, the absorption capacity of iodine can be detected by using a weighing method and an ultraviolet method.

9. Use of ionic liquids containing citrazinic acid anions according to claim 7 in iodine sorption, characterized in that: in the step 2), when the mixture I is dried by rotary evaporation, the mixture I is evaporated at the temperature of 80 ℃ for 10 hours and then is frozen and dried for 48 hours to obtain pure tetrabutylammonium citrazine salt ionic liquid; in the step 2), when the mixture I is dried in a vacuum drying oven, the drying temperature of 80 ℃ is kept for drying for 48 hours, and then the mixture is freeze-dried for 48 hours, so that pure tetrabutylammonium citrazinate ionic liquid is obtained.

10. The use of ionic liquids containing citrazinic acid anions according to claim 8, characterized in that: in the step 3), when absorbing iodine in the iodine vapor method, weighing citrazinic acid type ionic liquid, placing the citrazinic acid type ionic liquid in a plastic cover and at the bottom of a sealable reagent bottle, weighing solid iodine with a certain weight and placing the solid iodine in the sealable reagent bottle, wherein the solid iodine does not contact with the plastic cover containing the citrazinic acid type ionic liquid, sealing the reagent bottle and then placing the reagent bottle in an oven, heating the oven to 80 ℃ for 48 hours, and sublimating the solid iodine into iodine vapor and absorbing the iodine vapor by the citrazinic acid type ionic liquid in the plastic cover; in the step 3), when the citrazinic acid type ionic liquid absorbs iodine in the cyclohexane iodine solution, firstly, a certain weight of the citrazinic acid type ionic liquid is weighed and placed at the bottom of a test tube, solid iodine is added into the cyclohexane solution to prepare the cyclohexane iodine solution, and a certain weight of the cyclohexane iodine solution is weighed and added into the test tube containing the citrazinic acid type ionic liquid.

Technical Field

The invention relates to ionic liquid containing citrazinic acid anions and application thereof in iodine absorption, belonging to the field of chemical industry.

Background

The nuclear energy is a new energy source, and does not discharge carbon dioxide and nitrogen oxides into the atmosphere, so that the greenhouse effect is not increased, and the nuclear energy is clean and environment-friendly and is a clean and green new energy source. The energy density of nuclear energy is many times higher than that of fossil energy, hydrogen energy, wind energy, geothermal energy and the like, so that the efficiency of the nuclear energy is high. However, in the process of nuclear energy exploitation, nuclear accidents occur and nuclear waste is discharged inevitably. Historically, the trilly nuclear accident in the united states, the chernobiley nuclear accident in the former soviet union, and the fukushima nuclear accident in japan revealed a large amount of nuclear substances causing a large loss to humans and the environment. The nuclear waste and the nuclear material should be efficiently treated.

Iodine includes radioactive iodine 129, iodine 131, iodine 123, iodine 125 in addition to conventional iodine 127. In 2017, the world health organization also listed radioactive iodine as a carcinogen. Nuclear waste and nuclear material contain radioactive iodine. Moreover, the radioactive life of radioactive iodine is long, e.g., the half-life of iodine 129 is as long as 1590 ten thousand years. This means that the environmental and human hazards of radioactive iodine will be long-lived, which is one of the reasons why the adverse effects of nuclear waste discharged from the chernobyl nuclear event of the former soviet union and the fukushima nuclear accident of japan have not been eliminated so far. Therefore, it is important to absorb radioactive iodine.

In the traditional iodine absorption method, harmful materials such as heavy metal and the like are used for absorbing iodine, the absorption and synthesis steps are complex, the cost is high, and the large-scale utilization of iodine absorption is not facilitated.

Disclosure of Invention

The ionic liquid is salt which is composed of anions and cations and is liquid at the room temperature, has low volatility, strong stability, high designability and wide liquid range, and is an ideal green solvent and designable solvent for iodine absorption. The method for absorbing iodine by using the ionic liquid is simple, easy to operate, low in price, environment-friendly and high in practical application value.

The invention adopts the technical scheme that the ionic liquid containing the citrazinic acid anion has a chemical structural formula shown in a formula (1) or (2):

preferably, the ionic liquid containing the citrazinic acid anion is prepared by mixing citrazinic acid and tetrabutylammonium hydroxide, and the ionic liquid of formula (2) is prepared by mixing citrazinic acid and tetrabutylphosphorus hydroxide.

The application of ionic liquid containing citrazinic acid anions in iodine absorption comprises the following steps:

1) stirring and mixing citrazinic acid and an alkaline substance according to a certain molar ratio under a certain condition to obtain a first mixture;

2) drying the mixture I prepared in the step 1) to obtain citrazinic acid type ionic liquid;

3) absorbing iodine by the citrazinic acid type ionic liquid prepared in the step 2) under a certain condition;

4) taking the mixture of the ionic liquid and iodine prepared in the step 3), and detecting the absorption capacity of iodine in the ionic liquid.

Preferably, the ionic liquid containing the citrazinic acid anions is applied to iodine absorption, and in the step 1), the molar ratio of the citrazinic acid to the basic substance in the first mixture is 1:1 to 1: 3. .

Preferably, in the application of the ionic liquid containing the citrazinic acid anions in iodine absorption, in the step 1), the alkaline substance can be one or a mixture of more of tetrabutyl phosphorus hydroxide aqueous solution, tetrabutyl ammonium hydroxide aqueous solution and tetraethyl ammonium hydroxide aqueous solution; the mass fraction of the alkaline substance in the aqueous solution is 10 to 40 percent.

Preferably, in the application of the ionic liquid containing the citrazinic acid anions in iodine absorption, in the step 1), when the citrazinic acid and the alkaline substance are stirred and mixed according to a molar ratio, the mixing temperature is kept between 30 and 90 ℃, and the stirring and mixing time is 10 hours.

Preferably, when the mixture prepared in step 1) is dried in step 2), the drying method may be one or more of vacuum oven drying, rotary evaporation drying and freeze drying.

Optimally, the ionic liquid containing the citrazinic acid anions is applied to iodine absorption, in the step 3), when the citrazinic acid type ionic liquid absorbs iodine under a certain condition, the absorption condition can be that iodine is prepared into iodine vapor or iodine is prepared into a cyclohexane iodine solution; in step 4), when the absorption capacity of iodine in the ionic liquid is detected, the absorption capacity of iodine can be detected by using a weighing method and an ultraviolet method.

Optimally, the ionic liquid containing the citrazinic acid anions is applied to iodine absorption, and in the step 2), when the mixture I is dried by rotary evaporation, the mixture I is evaporated at the temperature of 80 ℃ for 10 hours and then is frozen and dried for 48 hours to obtain pure tetrabutylammonium citrazinate ionic liquid; in the step 2), when the mixture I is dried in a vacuum drying oven, the drying temperature of 80 ℃ is kept for drying for 48 hours, and then the mixture is freeze-dried for 48 hours, so that pure tetrabutylammonium citrazinate ionic liquid is obtained.

Optimally, when the citrazinic acid type ionic liquid absorbs iodine in an iodine vapor method, the citrazinic acid type ionic liquid is weighed and placed in a plastic cover and placed at the bottom of a sealable reagent bottle, solid iodine with a certain weight is weighed and placed in the sealable reagent bottle, the solid iodine does not contact with the plastic cover containing the citrazinic acid type ionic liquid, the reagent bottle is sealed and placed in an oven, the oven is heated to 80 ℃ and heated for 48 hours, and at the moment, the solid iodine is sublimated into iodine vapor and is absorbed by the citrazinic acid type ionic liquid in the plastic cover; in the step 3), when the citrazinic acid type ionic liquid absorbs iodine in the cyclohexane iodine solution, firstly, a certain weight of the citrazinic acid type ionic liquid is weighed and placed at the bottom of a test tube, solid iodine is added into the cyclohexane solution to prepare the cyclohexane iodine solution, and a certain weight of the cyclohexane iodine solution is weighed and added into the test tube containing the citrazinic acid type ionic liquid.

In the technical scheme of the application, the citrazinic acid type ionic liquid is prepared by mixing citrazinic acid and an alkaline substance and then drying, the preparation method is simple and convenient, and the ionic liquid is an ideal green solvent for iodine absorption. Citrazinic acid, tetrabutyl phosphorus hydroxide, tetrabutyl ammonium hydroxide and tetraethyl ammonium hydroxide which are citrazinic acid type ionic liquids are low in price and environment-friendly. The citrazinic acid type ionic liquid has high iodine absorption rate, is simple and convenient to absorb and operate, and has high practical application value

Drawings

Fig. 1(a) is a chemical structural formula (1) of the citrazinic acid ionic liquid, and fig. 1(b) is a chemical structural formula (2) of the citrazinic acid ionic liquid;

fig. 2 is an EDX energy spectrum of the citrazinic acid type ionic liquid of the present application;

FIG. 3 shows the relative mass fractions, theoretical relative mass fractions and errors of four elements, namely carbon, nitrogen, oxygen and phosphorus, in an EDX energy spectrum of the citrazinic acid type ionic liquid.

Detailed Description

The technical features of the present invention will be further explained with reference to the accompanying drawings and specific embodiments.