CN113372752A - High-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty and preparation method thereof - Google Patents
High-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty and preparation method thereof Download PDFInfo
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- CN113372752A CN113372752A CN202110887236.1A CN202110887236A CN113372752A CN 113372752 A CN113372752 A CN 113372752A CN 202110887236 A CN202110887236 A CN 202110887236A CN 113372752 A CN113372752 A CN 113372752A
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- flame
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- retardant
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/34—Filling pastes
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F1/00—Shielding characterised by the composition of the materials
- G21F1/02—Selection of uniform shielding materials
- G21F1/10—Organic substances; Dispersions in organic carriers
- G21F1/103—Dispersions in organic carriers
Abstract
The invention discloses high-temperature-resistant shielding putty with high flame retardance and high bonding strength and a preparation method thereof. The high-temperature-resistant shielding putty not only meets the requirement of high temperature resistance, but also has good shielding performance, flame retardance and bonding functions, the thermal weight loss of the material can be less than 4 percent when the material is continuously used for 300 days at 160 ℃, and the radiation shielding and structural safety performance under the severe condition can be met.
Description
Technical Field
The invention relates to the technical field of nuclear radiation protection, in particular to high-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty and a preparation method thereof.
Background
In the radiation protection design of nuclear facilities, the shields are spliced when the shields are constructed around the radioactive source. Due to the difference of the position and the structure, gaps with irregular shapes and structures can appear in the splicing process, and shielding putty needs to be adopted for filling and bonding so as to ensure the structural stability and the radiation protection safety of the radiation protection cable. Meanwhile, the flame-retardant cable is required to have good flame retardance and good thermal stability in many shielding occasions, and the risk of fire is prevented. Therefore, in addition to the requirement for flame retardancy of the shielding material itself, high flame retardancy and high adhesion strength are also required for the shielding putty.
The bonding strength of the shielding putty in the field of nuclear radiation protection is lower and is 0.5-2 MPa, the structural stability and the safety of the material are difficult to ensure in the use working condition, the splicing stability of a shielding body cannot be ensured, and the requirements of certain special devices or accessories are difficult to meet. In addition, in order to meet the high temperature resistance of the existing high temperature resistant shielding putty, the shielding putty is usually prepared by adopting an additive with higher use temperature, but in the field of nuclear radiation protection, the high temperature resistant shielding putty not only meets the requirement of high temperature resistance, but also needs to have good shielding performance and flame retardant and bonding functions.
Disclosure of Invention
The invention aims to provide the high-temperature-resistant shielding putty with high flame retardance and high bonding strength, and the prepared high-temperature-resistant shielding putty not only meets the requirement of high temperature resistance, but also has good shielding performance, flame retardance and bonding functions through reasonable design of a formula.
In addition, the invention also provides a preparation method of the high-temperature-resistant shielding putty
The invention is realized by the following technical scheme:
the high-flame-retardance high-adhesion-strength high-temperature-resistant shielding putty comprises a base body, a gamma-ray shielding filler, a neutron-ray shielding filler, a flame retardant and a curing agent, wherein the base body is epoxy resin, the flame retardant is aluminum hydroxide, and the curing agent is alicyclic amine.
The materials of the present invention, for example, alicyclic amines and the like, are commercially available.
The bonding strength of the shielding putty in the field of nuclear radiation protection is low, 0.5-2 MPa, the structural stability and safety of the material are difficult to ensure in the use working condition, the splicing stability of a shielding body cannot be ensured, and the requirements of certain special devices or accessories are difficult to meet.
Meanwhile, in order to meet the requirements of some special working conditions, the shielding putty for the nuclear radiation shielding field meets the basic shielding performance, high bonding strength, high-spacing flame retardance and high-temperature resistance.
Therefore, for the shielding putty in the field of nuclear radiation shielding, a flame retardant is required to be added on the premise of not influencing the shielding performance and the bonding strength of the shielding putty, so that the flame retardant effect is achieved, and the high-temperature resistance performance of the shielding putty is improved by adopting a high-temperature resistant curing agent.
Magnesium hydroxide and aluminum hydroxide are both additives used in shielding materials and can provide flame retardant properties, however, not all flame retardants are suitable for nuclear radiation shielding applications, such as: the flame retardant is added with magnesium hydroxide as a flame retardant, volatile water is generated into magnesium carbonate in the using process of the flame retardant, so that the neutron moderating performance and the flame retardant performance of the shielding material are gradually reduced, the technical requirements under severe conditions are difficult to meet, and the shielding requirement in the field of nuclear radiation cannot be met.
In order to improve the high temperature resistance of the shielding material, aniline curing agents with high temperature resistance are generally adopted in the prior art, and in the test process, the applicant finds that the aniline curing agents have low hydrogen content although the use temperature is high, and are adverse to the neutron moderation performance of the shielding material, and alicyclic amines with high heat resistance are used as the curing agents, are commercially available, have high hydrogen content and excellent heat resistance, can resist high temperature, and do not influence the neutron moderation performance of the shielding material.
In conclusion, the high-temperature-resistant shielding putty prepared by adopting the epoxy resin (EP) as a matrix, the aluminum hydroxide as a flame retardant, the high-heat-resistant alicyclic amine as a curing agent and the gamma-ray shielding filler and the neutron-ray shielding filler has the advantages of high temperature resistance, good shielding performance, flame retardance and bonding function, and the thermal weight loss of the material is less than 4% after the material is continuously used for 300 days at 160 ℃.
Furthermore, the weight percentage of the neutron ray shielding filler is 1 to 10 percent, the weight percentage of the gamma ray shielding filler is 60 to 80 percent, the weight percentage of the flame retardant is 4 to 30 percent, and the rest is the matrix and the curing agent.
The applicant finds through experiments that the shielding material prepared according to the proportion not only meets the requirement of high temperature resistance, but also has good shielding performance, flame retardance and bonding functions.
Furthermore, the weight percentage of the neutron ray shielding filler is 5 wt% -10 wt%, the weight percentage of the gamma ray shielding filler is 60 wt% -80 wt%, and the weight percentage of the flame retardant is 4 w% t% -15 wt%.
Furthermore, the dosage ratio of the matrix to the curing agent is 4.5: 1-3: 1, and the ratio of the resin to the curing agent can be adjusted according to the use requirement.
Further, the gamma ray shielding filler is lead powder.
Further, the neutron ray shielding filler is boron carbide.
A preparation method of high-flame-retardant and high-adhesion-strength high-temperature-resistant shielding putty comprises the following steps:
s1, adding the matrix and the flame retardant into a vacuum mixing system, and uniformly stirring;
s2, adding gamma-ray shielding filler and neutron-ray shielding filler, and stirring uniformly under a vacuum condition;
and S3, adding a curing agent, and continuously stirring for 0.5-1.5 h in vacuum to obtain the high-temperature-resistant shielding putty.
By adopting the formula and the process technology, the high-temperature-resistant shielding putty with excellent shielding performance, thermal stability, flame retardance and bonding performance can be prepared, and the radiation shielding and safety performance under severe conditions can be met.
Further, the vacuum degree in the stirring process is 1-2 Pa.
Further, the stirring speed is 30-70 r/min.
Furthermore, the weight percentage of the neutron ray shielding filler is 1 to 10 percent, the weight percentage of the gamma ray shielding filler is 60 to 80 percent, the weight percentage of the flame retardant is 4 to 30 percent, and the rest is the matrix and the curing agent.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the shielding putty prepared by the invention has excellent flame retardant property, bonding property and good thermal stability, can play a role of fire prevention, can be used for a long time at a high temperature of 160 ℃, and can meet the working condition requirement under a severe condition.
2. The formula and the component selection of the invention give consideration to shielding performance, thermal performance, flame retardant performance and bonding strength, and can provide excellent comprehensive performance so as to ensure protection safety and structural safety.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1:
the high-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty comprises the following components in percentage by weight:
16.35 wt% of epoxy resin, 60 wt% of lead powder, 5.11 wt% of boron carbide, 4.54 wt% of alicyclic amine and 14 wt% of aluminum hydroxide.
The preparation process comprises the following steps:
s1, adding the epoxy resin and the aluminum hydroxide into a vacuum mixing system in proportion, stirring at the speed of 30r/min for 10min, and stirring uniformly;
s2, adding lead powder and boron carbide, and stirring at the speed of 30r/min for 20min under a vacuum condition to be uniformly stirred;
s3, adding aluminum hydroxide, continuously stirring at the speed of 70r/min for 30min, and pouring according to different construction requirements or joint filling structure requirements;
the vacuum degree in the stirring process of the steps S1-S3 is 1-2 Pa.
Example 2:
the high-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty comprises the following components in percentage by weight:
7.825 wt% of epoxy resin, 80 wt% of lead powder, 5.47 wt% of boron carbide, 1.815 wt% of alicyclic amine and 4.89 wt% of aluminum hydroxide.
The preparation process comprises the following steps:
s1, adding the epoxy resin and the aluminum hydroxide into a vacuum mixing system in proportion, stirring at the speed of 30r/min for 10min, and stirring uniformly;
s2, adding lead powder and boron carbide, and stirring at the speed of 40r/min for 20min under a vacuum condition to be uniformly stirred;
s3, adding aluminum hydroxide, continuously stirring at the speed of 60r/min for 30min, and pouring according to different construction requirements or joint filling structure requirements;
the vacuum degree in the stirring process of the steps S1-S3 is 1-2 Pa.
Example 3:
the present example is based on example 1 and differs from example 1 in that it consists of, in weight percent:
16 wt% of epoxy resin, 60 wt% of lead powder, 10 wt% of boron carbide, 4 wt% of alicyclic amine and 10 wt% of aluminum hydroxide.
Example 4:
the present example is based on example 1 and differs from example 1 in that it consists of, in weight percent:
12 wt% of epoxy resin, 60 wt% of lead powder, 4 wt% of boron carbide, 4 wt% of alicyclic amine and 20 wt% of aluminum hydroxide.
Comparative example 1:
this comparative example is based on example 1 and differs from example 1 in that:
equal amounts of magnesium hydroxide were used instead of aluminum hydroxide.
Comparative example 2:
this comparative example is based on example 1 and differs from example 1 in that:
the alicyclic amine was replaced with an equivalent amount of aniline curing agent.
Comparative example 3:
this comparative example is based on example 1 and differs from example 1 in that:
the aluminum hydroxide was replaced with an equal amount of magnesium hydroxide and the alicyclic amine was replaced with an equal amount of aniline curing agent.
Comparative example 4:
this comparative example is based on example 1 and differs from example 1 in that: the dosage of each component is different, and the specific dosage is as follows:
the paint comprises the following components in percentage by weight:
16.35 wt% of epoxy resin, 71 wt% of lead powder, 5.11 wt% of boron carbide, 4.54 wt% of alicyclic amine and 3 wt% of aluminum hydroxide.
Comparative example 5:
this comparative example is based on example 1 and differs from example 1 in that: the dosage of each component is different, and the specific dosage is as follows:
the paint comprises the following components in percentage by weight:
16.35 wt% of epoxy resin, 73 wt% of lead powder, 5.11 wt% of boron carbide, 4.54 wt% of alicyclic amine and 1 wt% of aluminum hydroxide.
Comparative example 6:
this comparative example is based on example 1 and differs from example 1 in that: the dosage of each component is different, and the specific dosage is as follows:
the paint comprises the following components in percentage by weight:
13 wt% of epoxy resin, 60 wt% of lead powder, 5 wt% of boron carbide, 12 wt% of alicyclic amine and 10 wt% of aluminum hydroxide.
Comparative example 7:
this comparative example is based on example 1 and differs from example 1 in that: the dosage of each component is different, and the specific dosage is as follows:
the paint comprises the following components in percentage by weight:
21 wt% of epoxy resin, 60 wt% of lead powder, 5 wt% of boron carbide, 4 wt% of alicyclic amine and 10 wt% of aluminum hydroxide.
And (3) testing the application effect: preparing shielding putty according to the formulas of example 1-example 3, comparative example 1-comparative example 7; a series of related performance tests are carried out according to the national standard, and the test result shows that the prepared shielding putty has excellent performances. Specific indexes are shown in table 1:
TABLE 1
From the data in table 1, it can be seen that:
1) the invention takes epoxy resin as a matrix material, lead powder and boron carbide as shielding material fillers, aluminum hydroxide as a flame retardant to enhance the flame retardant property, and alicyclic amine with high heat resistance as a curing agent to enhance the bonding property and the thermal stability. The prepared shielding putty has the advantages of short surface drying and actual drying time, low shrinkage rate, excellent flame retardant property, high bonding strength, excellent gamma, thermal neutron and fast neutron shielding properties, thermal weight loss of less than 4% after being continuously used for 300 days at 160 ℃, and can ensure the radiation safety of equipment and personnel and the working condition requirement under severe conditions.
2) When magnesium hydroxide is used for replacing aluminum hydroxide, the fast neutron shielding coefficient and the oxygen index of the prepared shielding putty material are reduced, because magnesium hydroxide is used as a flame retardant and generates magnesium carbonate by volatile water in the using process.
3) When the alicyclic amine is replaced by the aniline curing agent, the surface drying time and the actual drying time of the prepared shielding putty material are increased, because the curing temperature required by taking the aniline as the curing agent is higher; the fast neutron shielding coefficient is reduced because the aniline as the curing agent contains lower hydrogen content.
4) Meanwhile, magnesium hydroxide is used for replacing aluminum hydroxide, and aniline curing agent is used for replacing alicyclic amine, so that the surface drying time and the actual drying time of the prepared shielding putty material are increased, and the fast neutron shielding coefficient and the oxygen index are reduced.
5) When the using amount of the aluminum hydroxide is lower than the range of the invention, the oxygen index of the prepared shielding putty material is greatly reduced, and the flame retardant property is sharply reduced; above the range of the present invention, the addition of the neutron ray shielding filler is affected, thereby affecting the thermal neutron shielding performance.
6) When the proportion of the resin and the curing agent is out of the range of the invention, the surface drying time and the actual drying time of the prepared shielding putty material are greatly increased, and meanwhile, the bonding strength is obviously reduced, which is not beneficial to the requirements of the working conditions used by the material.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The high-flame-retardance high-adhesion-strength high-temperature-resistant shielding putty comprises a base body, gamma-ray shielding filler, neutron-ray shielding filler, a flame retardant and a curing agent, and is characterized in that the base body is epoxy resin, the flame retardant is aluminum hydroxide, and the curing agent is alicyclic amine.
2. The high-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty as claimed in claim 1, wherein the weight percentage of neutron ray shielding filler is 1-10 wt%, the weight percentage of gamma ray shielding filler is 60-80 wt%, the weight percentage of flame retardant is 4-30 wt%, and the balance is matrix and curing agent.
3. The high flame retardant and high adhesion strength high temperature resistant shielding putty as claimed in claim 2, wherein the weight percentage of the neutron ray shielding filler is 5 wt% -10 wt%, the weight percentage of the gamma ray shielding filler is 60 wt% -80 wt%, and the weight percentage of the flame retardant is 4 w% t% -15 wt%.
4. The high-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty as claimed in claim 2, wherein the dosage ratio of the matrix to the curing agent is 4.5: 1-3: 1.
5. The high-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty as claimed in claim 1, wherein the gamma-ray shielding filler is lead powder.
6. The high-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty as claimed in claim 1, wherein the neutron ray shielding filler is boron carbide.
7. The method for preparing high-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty as claimed in any one of claims 1 to 6, which is characterized by comprising the following steps:
s1, adding the matrix and the flame retardant into a vacuum mixing system, and uniformly stirring;
s2, adding gamma-ray shielding filler and neutron-ray shielding filler, and stirring uniformly under a vacuum condition;
and S3, adding a curing agent, and continuously stirring for 0.5-1.5 h in vacuum to obtain the high-temperature-resistant shielding putty.
8. The preparation method of the high-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty as claimed in claim 7, wherein the vacuum degree in the stirring process is 1-2 Pa.
9. The preparation method of the high-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty as claimed in claim 7, wherein the stirring speed is 30-70 r/min.
10. The preparation method of the high flame-retardant high-bonding-strength high-temperature-resistant shielding putty as claimed in claim 7, wherein the weight percentage of the neutron ray shielding filler is 1 wt% -10 wt%, the weight percentage of the gamma ray shielding filler is 60 wt% -80 wt%, the weight percentage of the flame retardant is 4 w% t% -30 wt%, and the balance is a base body and a curing agent.
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| CN202110887236.1A CN113372752A (en) | 2021-08-03 | 2021-08-03 | High-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty and preparation method thereof |
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| CN202110887236.1A CN113372752A (en) | 2021-08-03 | 2021-08-03 | High-flame-retardant high-adhesion-strength high-temperature-resistant shielding putty and preparation method thereof |
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