A method for solidifying waste scintillating liquid and a solidifying agent thereof

The curing reaction of epoxy resin and ethylenediamine forms a solidified body of the waste scintillation liquid, which solves the safety hazards and environmental risks of the waste scintillation liquid, and achieves the effect of stabilizing curing and reducing transportation risks.

CN115602350BActive Publication Date: 2025-08-29THE 404 COMPANY LIMITED CHINA NAT NUCLEAR
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Patent Information

Application Number
CN202211247318.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-10-12
Publication Date
2025-08-29
Estimated Expiration
2042-10-12

AI Technical Summary

Technical Problem

In the prior art, waste scintillation liquid is highly toxic and flammable. It has safety hazards and environmental risks in long-term storage or transportation, and is difficult to recycle and deal with, resulting in high environmental pollution risks.

Method used

A curing agent of epoxy resin and ethylenediamine is used to form a cured body by stirring and mixing and curing reaction, which envelops the waste scintillation liquid to form a stable cured body.

Benefits of technology

The stable curing of waste scintillation liquid is achieved, which reduces safety risks in storage and transportation, and reduces environmental risks. The formed cured body has good hardness and anti-leaching properties.

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Abstract

The present invention provides a method for curing waste scintillating liquid and a curing agent thereof. The method comprises: taking the waste scintillating liquid, adding epoxy resin, and then adding ethylenediamine to the waste scintillating liquid, and forming a solidified body of the waste scintillating liquid through a curing reaction. The method of the present invention can achieve the curing treatment of the waste scintillating liquid, and the resulting solidified body has good stability, good hardness, no fluidity, and good leaching resistance, which can significantly reduce safety hazards and risks during storage and transportation.
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Description

Technical Field

[0001] The present invention relates to the technical field of radioactive waste treatment, in particular to a method for solidifying waste scintillating liquid and a solidifying agent thereof. Background Art

[0002] Liquid scintillation counting is one of the important analytical methods for determining the α / β radioactivity in radioactive samples. 3 H. 63 Ni, 14 C. 90 Sr. 99 Tc, 55 The measurement of radionuclides such as Fe has been widely used in nuclear medicine, nuclear technology, radiation environmental monitoring, biology, and other fields. With the further development of liquid scintillation counting technology, the number of samples analyzed has increased dramatically, consuming a large amount of scintillation fluid and resulting in a large accumulation of waste scintillation fluid. Waste scintillation fluid is highly toxic and flammable, posing significant safety and environmental risks during long-term storage or transportation. Once a leak occurs, it is difficult to recover, causing local environmental pollution and making subsequent environmental pollution control difficult and costly.

[0003] In view of this, the treatment and disposal of waste scintillation fluid needs to be solved urgently. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide a method for solidifying waste scintillating liquid and a solidifying agent thereof, so as to solve the technical problem that waste scintillating liquid generated by liquid scintillation counting method in the prior art has potential safety hazards and environmental risks.

[0005] In order to solve the above technical problems, the technical solutions of the present invention are as follows:

[0006] A method for solidifying waste scintillating liquid, comprising:

[0007] Take the waste scintillating liquid, add epoxy resin, and then add ethylenediamine to the waste scintillating liquid to form a solidified body of the waste scintillating liquid through a curing reaction.

[0008] Preferably, 3-8 g of the epoxy resin and 0.5-2 g of the ethylenediamine are added to every 10 ml of the waste scintillation fluid.

[0009] Preferably, the method for solidifying the waste scintillating liquid specifically comprises:

[0010] Take the waste scintillating liquid, add epoxy resin, stir for 3-10 minutes, then add ethylenediamine, stir for 5-20 minutes, and form a solidified body of the waste scintillating liquid through a curing reaction.

[0011] Preferably, the reaction temperature of the curing reaction is 25-50° C., and the reaction time is 20-36 hours.

[0012] Preferably, the epoxy resin is one or more of a condensation product of epichlorohydrin and bisphenol A, and a condensation product of epichlorohydrin and polyol.

[0013] Preferably, the polyol is one or more of pentaerythritol, ethylene glycol, glycerol, and dichloropropane.

[0014] Preferably, the waste scintillation liquid uses one or more of diisopropyl alkane and dioxane as solvent.

[0015] The invention provides a curing agent for waste scintillating liquid, comprising epoxy resin and ethylenediamine.

[0016] Preferably, the mass ratio of the epoxy resin to the ethylenediamine is (3-8):1.

[0017] Preferably, the mass ratio of the epoxy resin to the ethylenediamine is 7.5:1.

[0018] The above solution of the present invention includes at least the following beneficial effects:

[0019] (1) The method for curing waste scintillating liquid of the present invention comprises: taking waste scintillating liquid, adding epoxy resin, and then adding ethylenediamine thereto, and forming a solidified body of the waste scintillating liquid through a curing reaction. The method of the present invention can achieve the curing treatment of the waste scintillating liquid, and the formed solidified body has good stability, good hardness, no fluidity, and good anti-leaching performance, which can greatly reduce safety hazards and reduce safety risks during storage and transportation.

[0020] (2) The method for curing the waste scintillating liquid of the present invention comprises the following steps: after mixing the waste scintillating liquid with epoxy resin, ethylenediamine is added. The active hydrogen in ethylenediamine causes the epoxy groups in the epoxy resin to open the ring and cross-link with ethylenediamine to form a three-dimensional network polymer. The waste scintillating liquid is encapsulated in the three-dimensional network to form a solidified product. DETAILED DESCRIPTION

[0021] In the examples of the present invention, if specific conditions are not specified, the experiments were carried out under conventional conditions or the conditions recommended by the manufacturer. Reagents or instruments used without specifying the manufacturer are all commercially available conventional products. Raw materials of different manufacturers and types do not affect the implementation of the technical solutions of the present invention and the achievement of the technical effects.

[0022] Example 1

[0023] The curing agent for the waste scintillating liquid used in this embodiment includes epoxy resin and ethylenediamine, wherein the mass ratio of the epoxy resin to the ethylenediamine is 3:1.

[0024] The method for solidifying the waste scintillating liquid of this embodiment includes:

[0025] Take the waste scintillating liquid, add epoxy resin, stir for 5 minutes, then add ethylenediamine, stir for 5 minutes, and undergo curing reaction at a reaction temperature of 25° C. and a reaction time of 36 hours to form a solidified body of the waste scintillating liquid.

[0026] Wherein, 3g of the epoxy resin and 1g of the ethylenediamine are added to every 10ml of the waste scintillation fluid. The epoxy resin is a condensation product of epichlorohydrin and bisphenol A.

[0027] In this embodiment, the waste scintillating fluid uses diisopropyl alkane and dioxane as solvents. It should be noted that for the purposes of the present invention, the composition of the waste scintillating fluid is not limited. This embodiment uses waste scintillating fluid containing diisopropyl alkane and dioxane as an example for solidification treatment. Those skilled in the art may also substitute waste scintillating fluids with other compositions, depending on the actual situation.

[0028] Example 2

[0029] The curing agent for the waste scintillating liquid used in this embodiment includes epoxy resin and ethylenediamine, wherein the mass ratio of the epoxy resin to the ethylenediamine is 8:1.

[0030] The method for solidifying the waste scintillating liquid of this embodiment includes:

[0031] Take the waste scintillating liquid, add epoxy resin, stir for 3 minutes, then add ethylenediamine, stir for 12 minutes, and undergo a curing reaction at a reaction temperature of 50° C. and a reaction time of 24 hours to form a solidified body of the waste scintillating liquid.

[0032] 8 g of the epoxy resin and 1 g of ethylenediamine were added to every 10 ml of the waste scintillation fluid. The epoxy resin was a condensation product of epichlorohydrin and a polyol. The polyol was ethylene glycol.

[0033] In this embodiment, the waste scintillating fluid uses diisopropyl alkane and dioxane as solvents. It should be noted that for the purposes of the present invention, the composition of the waste scintillating fluid is not limited. This embodiment uses waste scintillating fluid containing diisopropyl alkane and dioxane as an example for solidification treatment. Those skilled in the art may also substitute waste scintillating fluids with other compositions, depending on the actual situation.

[0034] Example 3

[0035] The curing agent for the waste scintillating liquid used in this embodiment includes epoxy resin and ethylenediamine, wherein the mass ratio of the epoxy resin to the ethylenediamine is 4:1.

[0036] The method for solidifying the waste scintillating liquid of this embodiment includes:

[0037] Take the waste scintillating liquid, add epoxy resin, stir for 10 minutes, then add ethylenediamine, stir for 20 minutes, and undergo curing reaction at a reaction temperature of 30° C. and a reaction time of 20 hours to form a solidified body of the waste scintillating liquid.

[0038] Wherein, 8g of the epoxy resin and 2g of ethylenediamine are added to every 10ml of the waste scintillation fluid. The epoxy resin is a condensation product of epichlorohydrin and a polyol. The polyol is glycerol.

[0039] In this embodiment, the waste scintillating fluid uses diisopropyl alkane and dioxane as solvents. It should be noted that for the purposes of the present invention, the composition of the waste scintillating fluid is not limited. This embodiment uses waste scintillating fluid containing diisopropyl alkane and dioxane as an example for solidification treatment. Those skilled in the art may also substitute waste scintillating fluids with other compositions, depending on the actual situation.

[0040] Example 4

[0041] The curing agent for the waste scintillating liquid used in this embodiment includes epoxy resin and ethylenediamine, wherein the mass ratio of the epoxy resin to the ethylenediamine is 7.5:1.

[0042] The method for solidifying the waste scintillating liquid of this embodiment includes:

[0043] Take the waste scintillating liquid, add epoxy resin, stir for 5 minutes, then add ethylenediamine, stir for 20 minutes, and undergo curing reaction at a reaction temperature of 30° C. and a reaction time of 20 hours to form a solidified body of the waste scintillating liquid.

[0044] Wherein, 7.5g of the epoxy resin and 1g of ethylenediamine are added to every 10ml of the waste scintillation fluid. The epoxy resin is a condensation product of epichlorohydrin and a polyol. The polyol is dichloropropane.

[0045] In this embodiment, the waste scintillating fluid uses diisopropyl alkane and dioxane as solvents. It should be noted that for the purposes of the present invention, the composition of the waste scintillating fluid is not limited. This embodiment uses waste scintillating fluid containing diisopropyl alkane and dioxane as an example for solidification treatment. Those skilled in the art may also substitute waste scintillating fluids with other compositions, depending on the actual situation.

[0046] Effect comparison ratio

[0047] In order to verify the technical effect of the method for solidifying waste scintillating liquid of the present invention, the following experiments were conducted:

[0048] Take the solidified waste scintillating liquid prepared in Examples 1-4, weigh it, and place it in a water bath. Set the water bath temperature to 30°C, 40°C, and 50°C, respectively. Heat the same solidified body at different temperature ranges for 30 minutes. Record the changes in the mass of the solidified body under different temperature conditions and the apparent properties of the solidified body after heating to determine the temperature stability of the solidified body.

[0049] After experimentation, the results are as follows:

[0050]

[0051] The solidified waste scintillating fluid prepared in Examples 1-4 was completely immersed in water, and the total α leaching rate and the total β leaching rate in the aqueous solution after immersion for 42 days were measured by liquid scintillation counting.

[0052] After experimentation, the results are as follows:

[0053] Group Total α leaching rate Total β leaching rate Example 1 <![CDATA[1.26×10 -8 ]]> <![CDATA[1.34×10 -7 ]]> Example 2 <![CDATA[2.06×10 -8 ]]> <![CDATA[1.56×10 -7 ]]> Example 3 <![CDATA[1.89×10 -8 ]]> <![CDATA[1.12×10 -7 ]]> Example 4 <![CDATA[1.20×10 -8 ]]> <![CDATA[1.11×10 -7 ]]>

[0054] From the above results, it can be seen that in the method for curing the waste scintillating liquid in Example 4, the mass ratio of the epoxy resin to the ethylenediamine is 7.5:1, and the epoxy resin is a condensation product of epichlorohydrin and dichloropropanol. The resulting cured body has better stability, good hardness, no fluidity, and optimal anti-leaching performance.

[0055] It is understood from common technical knowledge that the present invention may be implemented by other embodiments that do not depart from its spirit or essential features. Therefore, the embodiments disclosed above are, in all respects, merely illustrative and not exclusive. All modifications within the scope of the present invention or equivalent to the scope of the present invention are intended to be encompassed by the present invention.

Claims

1. A method for solidifying waste scintillating liquid, characterized in that: include: Taking waste scintillating liquid, adding epoxy resin, and then adding ethylenediamine thereto, and forming a solidified body of the waste scintillating liquid through a curing reaction; The epoxy resin is a condensation product of epichlorohydrin and a polyol; the polyol is one or more of pentaerythritol, ethylene glycol, glycerol, and dichloropropane; The reaction temperature of the curing reaction is 25-50°C and the reaction time is 20-36h; The mass ratio of the epoxy resin to the ethylenediamine is (3-8):

1.

2. The method for solidifying waste scintillating liquid according to claim 1, characterized in that: To every 10 ml of the waste scintillation fluid, 3-8 g of the epoxy resin and 0.5-2 g of the ethylenediamine were added.

3. The method for solidifying waste scintillating liquid according to claim 1, characterized in that: Specifically include: Take the waste scintillating liquid, add epoxy resin, stir for 3-10 minutes, then add ethylenediamine, stir for 5-20 minutes, and form a solidified body of the waste scintillating liquid through a curing reaction.

4. The method for solidifying waste scintillating liquid according to claim 1, characterized in that: The waste scintillation liquid uses one or more of diisopropyl alkane and dioxane as solvent.

5. A curing agent for waste scintillating liquid, characterized in that: include: Epoxy resin and ethylenediamine; the epoxy resin is a condensation product of epichlorohydrin and polyol; The polyol is one or more of pentaerythritol, ethylene glycol, glycerol, and dichloropropanol; the mass ratio of the epoxy resin to the ethylenediamine is (3-8):

1.

6. The curing agent for waste scintillating liquid according to claim 5, characterized in that The mass ratio of the epoxy resin to the ethylenediamine is 7.5:1.

Citation Information

Patent Citations

  • Method for solidifying radioactive waste

    WO2020222451A1