CN110964144A - Formula and preparation method of X-ray-proof glass - Google Patents

Formula and preparation method of X-ray-proof glass Download PDF

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Publication number
CN110964144A
CN110964144A CN201911318466.5A CN201911318466A CN110964144A CN 110964144 A CN110964144 A CN 110964144A CN 201911318466 A CN201911318466 A CN 201911318466A CN 110964144 A CN110964144 A CN 110964144A
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lead
ray
prepolymer
modifier
methacrylate
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Inventor
吴贲华
陈云
高国忠
袁厚呈
申云飞
王健
刘成彬
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Jiangsu Tiemao Glass Co Ltd
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Jiangsu Tiemao Glass Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098—Metal salts of carboxylic acids
    • 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
    • G21F1/06—Ceramics; Glasses; Refractories

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention relates to a formula of X-ray-proof glass and a preparation method thereof, wherein the formula comprises the following components in percentage by weight: 80% -90% of a prepolymer; 5% -19% of a modifier; and 1% -5% of an initiator. The preparation method comprises the following steps: taking 80-90% of prepolymer, 5-19% of modifier and 1-5% of initiator by weight percentage; adding the prepolymer into a reaction kettle, heating and stirring until the prepolymer is clear, and evaporating until the weight is constant; adding a modifier into a reaction kettle, vacuumizing, and reacting the modifier with a prepolymer to obtain a first clarified solution; adding an initiator into the first clarified solution, and stirring to obtain a second clarified solution; pouring the second clarified solution into a mould, and heating and curing; and cooling and then removing the mold to obtain the X-ray-proof glass. The X-ray-proof glass prepared by the invention has the advantages of high transparency, good toughness, high strength, light weight and difficult attenuation.

Description

Formula and preparation method of X-ray-proof glass
Technical Field
The invention relates to an X-ray-proof glass, in particular to a formula and a preparation method of the X-ray-proof glass.
Background
X-ray shielding glass is glass which contains sufficient heavy metals, such as lead, barium and the like, and can provide excellent X-ray protection for organisms. X-ray resistant glass allows the operator or observer to be protected from hazardous radiation.
In the process of implementing the invention, the inventor finds that the prior art has at least the following problems:
the prior art X-ray resistant glass is generally inorganic glass, is relatively weak and cannot be strengthened, resulting in it being fragile and therefore requiring great care in production, transportation, storage, installation and use, which is disadvantageous to its production, transportation, storage, installation and use.
Disclosure of Invention
In order to solve the technical problems in the prior art, the embodiment of the invention provides a formula and a preparation method of an X-ray-proof glass. The specific technical scheme is as follows:
in a first aspect, a formula of an X-ray-proof glass is provided, wherein the formula of the X-ray-proof glass comprises the following components in percentage by weight:
80% -90% of a prepolymer;
5% -19% of a modifier; and
1% -5% of initiator.
In a first possible implementation of the first aspect, the prepolymer is a mixture of methacrylic acid, methyl methacrylate, and a lead-containing compound.
In combination with the first possible implementation manner of the first aspect, in a second possible implementation manner of the first aspect, the lead-containing compound is one or more of basic lead carbonate, lead acetate trihydrate, lead acetate, lead nitrate, lead oxide, lead phosphate, lead sulfate, lead acetate, and lead bromide.
In combination with the first possible implementation manner of the first aspect, in a third possible implementation manner of the first aspect, the methacrylate is one or more of methyl methacrylate, ethyl methacrylate, and propyl methacrylate.
In a fourth possible implementation of the first aspect, the modifier is one or more of 2-hydroxyethyl methacrylate, neopentyl glycol, and boric acid.
In a fourth possible implementation of the first aspect, the initiator is one or more of tert-butyl peroxyneodecanoate, dibutyl peroxydicarbonate, tert-butyl peroxy2-ethylhexanoate, tert-butyl peroxyacetate, and 1,1,3, 3-tetramethylbutyl peroxypivalate.
In a second aspect, a method for preparing an X-ray resistant glass is provided, which comprises the following steps:
taking 80-90% of prepolymer, 5-19% of modifier and 1-5% of initiator by weight percentage;
adding the prepolymer into a reaction kettle, heating and stirring until the prepolymer is clear, and evaporating until the weight is constant;
adding a modifier into a reaction kettle, vacuumizing, and reacting the modifier with a prepolymer to obtain a first clarified solution;
adding an initiator into the first clarified solution, and stirring to obtain a second clarified solution;
pouring the second clarified solution into a mould, and heating and curing; and
and cooling and then removing the mold to obtain the X-ray-proof glass.
In a first possible implementation of the second aspect, the prepolymer is a mixture of methacrylic acid, methyl methacrylate and a lead-containing compound.
In combination with the first possible implementation manner of the second aspect, in a second possible implementation manner of the second aspect, the lead-containing compound is one or more of basic lead carbonate, lead acetate trihydrate, lead acetate, lead nitrate, lead oxide, lead phosphate, lead sulfate, lead acetate, and lead bromide; and/or the methacrylate is one or more of methyl methacrylate, ethyl methacrylate and propyl methacrylate.
In a third possible implementation of the second aspect, the modifier is one or more of 2-hydroxyethyl methacrylate, neopentyl glycol, and boric acid; and/or the initiator is one or more of tert-butyl peroxyneodecanoate, dibutyl peroxydicarbonate, tert-butyl peroxy2-ethylhexanoate, tert-butyl peroxyacetate and 1,1,3, 3-tetramethylbutyl peroxypivalate.
Compared with the prior art, the invention has the advantages that:
the anti-X-ray glass prepared by the invention is prepared by adding the radiation-proof element on the basis of an acrylic material and keeps some original characteristics of acrylic, so that the anti-X-ray glass prepared by the invention is acrylic anti-X-ray glass, also called organic glass (PMMA), and PMMA is a long-chain high polymer and has a very soft molecular chain, so that the strength of PMMA is higher, and the tensile and impact resistance capability of PMMA is 7-18 times higher than that of common glass, so that the anti-X-ray glass is not a fragile product, and the problem that the anti-X-ray glass in the prior art is easy to break in the using process can be effectively solved.
Meanwhile, the acrylic plate has good toughness, but the acrylic plate still has the bearing limit, and if the pressure borne by the acrylic plate exceeds the bearing limit, the acrylic plate can be broken, but cannot be broken into whole blocks to form slag like common glass, so that the X-ray-proof glass prepared by the invention is broken into particles even if being broken, is not easy to hurt people, and has high safety.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic flow chart of the steps of the method for preparing the X-ray-proof glass according to the first, second and third embodiments of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
In one embodiment of the invention, the following components are weighed according to the weight percentage of the formula: 15% methacrylic acid, 20% methyl methacrylate, 50% lead acetate trihydrate, 14.88% 2-hydroxyethyl methacrylate, and 0.12% t-butyl peroxy (2-ethylhexanoate).
Referring to fig. 1, a schematic flow chart of steps of a method 1 for manufacturing an X-ray shielding glass according to an embodiment of the invention is shown. The preparation method 1 of the X-ray-proof glass comprises the following steps 101-105, wherein:
step 101, heating and evaporating the prepolymer. And adding the weighed methacrylic acid, methyl methacrylate and lead-containing compound into a reaction kettle, heating and stirring until the mixture is clear and transparent, and evaporating until the weight is constant. Preferably, the temperature for heating and stirring is 70 ℃, but not limited thereto.
Step 102, adding a modifier. Adding a modifier into a reaction kettle, vacuumizing, reacting the modifier with the prepolymer, and obtaining a first clear solution after the modifier and the prepolymer are completely reacted.
Step 103, adding an initiator. And adding an initiator into the first clarified solution, wherein the initiator can react with the first clarified solution, stirring the solution, and obtaining a second clarified solution after the solution is fully reacted.
And 104, heating and curing. Pouring the second clarified solution into a mold with a thickness of 12mm, and heating and curing, wherein the heating temperature can be set to 70 ℃, the curing time can be set to 12 hours, the heating temperature can also be set to 100 ℃, and the curing time can be set to 4 hours, but the invention is not limited thereto.
And step 105, cooling and demolding. And cooling, removing the mold, and taking out the solidified second clear solution to obtain the X-ray-proof glass.
In the second embodiment of the invention, the components are weighed according to the weight percentage of the formula: 10% methacrylic acid, 14.5% methyl methacrylate, 0.5% ethyl methacrylate, 62% basic lead carbonate, 12.87% neopentyl glycol and 0.13% t-butyl peroxyacetate.
Referring to fig. 1, a schematic flow chart of steps of a method 1 for preparing an X-ray resistant glass according to two embodiments of the present invention is shown. The preparation method 1 of the X-ray-proof glass comprises the following steps 101-105, wherein:
step 101, heating and evaporating the prepolymer. And adding the weighed methacrylic acid, methyl methacrylate and lead-containing compound into a reaction kettle, heating and stirring until the mixture is clear and transparent, and evaporating until the weight is constant. Preferably, the temperature for heating and stirring is 70 ℃, but not limited thereto.
Step 102, adding a modifier. Adding a modifier into a reaction kettle, vacuumizing, reacting the modifier with the prepolymer, and obtaining a first clear solution after the modifier and the prepolymer are completely reacted.
Step 103, adding an initiator. And adding an initiator into the first clarified solution, wherein the initiator can react with the first clarified solution, stirring the solution, and obtaining a second clarified solution after the solution is fully reacted.
And 104, heating and curing. Pouring the second clarified solution into a mold with a thickness of 12mm, and heating and curing, wherein the heating temperature can be set to 70 ℃, the curing time can be set to 12 hours, the heating temperature can also be set to 100 ℃, and the curing time can be set to 4 hours, but the invention is not limited thereto.
And step 105, cooling and demolding. And cooling, removing the mold, and taking out the solidified second clear solution to obtain the X-ray-proof glass.
In the three embodiments of the invention, the following components are weighed according to the weight percentage of the formula: 10% methacrylic acid, 17% methyl methacrylate, 1% propyl methacrylate, 62% lead acetate, 9.84% boric acid and 0.16% t-butyl peroxy (2-ethylhexanoate).
Referring to fig. 1, a schematic flow chart of steps of a method 1 for preparing an X-ray resistant glass according to three embodiments of the present invention is shown. The preparation method 1 of the X-ray-proof glass comprises the following steps 101-105, wherein:
step 101, heating and evaporating the prepolymer. And adding the weighed methacrylic acid, methyl methacrylate and lead-containing compound into a reaction kettle, heating and stirring until the mixture is clear and transparent, and evaporating until the weight is constant. Preferably, the temperature for heating and stirring is 70 ℃, but not limited thereto.
Step 102, adding a modifier. Adding a modifier into a reaction kettle, vacuumizing, reacting the modifier with the prepolymer, and obtaining a first clear solution after the modifier and the prepolymer are completely reacted.
Step 103, adding an initiator. And adding an initiator into the first clarified solution, wherein the initiator can react with the first clarified solution, stirring the solution, and obtaining a second clarified solution after the solution is fully reacted.
And 104, heating and curing. Pouring the second clarified solution into a mold with a thickness of 12mm, and heating and curing, wherein the heating temperature can be set to 70 ℃, the curing time can be set to 12 hours, the heating temperature can also be set to 100 ℃, and the curing time can be set to 4 hours, but the invention is not limited thereto.
And step 105, cooling and demolding. And cooling, removing the mold, and taking out the solidified second clear solution to obtain the X-ray-proof glass.
The properties of the X-ray shielding glass prepared in one to three examples and the X-ray shielding glass of the prior art were tested in four groups, wherein each group of test items comprises tensile strength (ASTM D638), tensile modulus (ASTM D638), impact strength (simple beam) GB/T1043, heat distortion temperature ASTM D648, transmittance and haze ASTM 1003.
A first group: the test object was the X-ray resistant glass prepared in one example, and the test results were as follows:
Figure BDA0002326494280000071
second group: the test object is the X-ray-proof glass prepared in the two examples, and the test results are as follows:
Figure BDA0002326494280000072
third group: the test object was the X-ray-proof glass prepared in the three examples, and the test results were as follows:
Figure BDA0002326494280000073
Figure BDA0002326494280000081
third group: the test object is the X-ray-proof glass in the prior art, and the test results are as follows:
Figure BDA0002326494280000082
by combining the first to third groups of test data and the fourth group of test data, the X-ray-proof glass can be obviously obtained, and by using the formula and the preparation method of the X-ray-proof glass, the prepared X-ray-proof glass has the advantages of high transparency, good toughness, high strength, light weight and low attenuation tendency.
The foregoing description shows and describes several preferred embodiments of the invention, but as aforementioned, it is to be understood that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. The formula of the X-ray-proof glass is characterized by comprising the following components in percentage by weight:
80% -90% of a prepolymer;
5% -19% of a modifier; and
1% -5% of initiator.
2. The formulation for an X-ray resistant glass according to claim 1, wherein the prepolymer is a mixture of methacrylic acid, methyl methacrylate and a lead-containing compound.
3. The formulation for an X-ray resistant glass according to claim 2, wherein the lead-containing compound is one or more of basic lead carbonate, lead acetate trihydrate, lead acetate, lead nitrate, lead oxide, lead phosphate, lead sulfate, lead acetate, and lead bromide.
4. The formulation of an X-ray resistant glass according to claim 2, wherein the methacrylate is one or more of methyl methacrylate, ethyl methacrylate and propyl methacrylate.
5. The formulation for an X-ray resistant glass according to claim 1, wherein the modifier is one or more of 2-hydroxyethyl methacrylate, neopentyl glycol and boric acid.
6. The formulation for X-ray resistant glass according to claim 1, wherein the initiator is one or more of t-butyl peroxyneodecanoate, dibutyl peroxydicarbonate, t-butyl peroxy (2-ethylhexanoate), t-butyl peroxyacetate and 1,1,3, 3-tetramethylbutyl peroxypivalate.
7. The preparation method of the X-ray-proof glass is characterized by comprising the following steps of:
taking 80-90% of prepolymer, 5-19% of modifier and 1-5% of initiator by weight percentage;
adding the prepolymer into a reaction kettle, heating and stirring until the prepolymer is clear, and evaporating until the weight is constant;
adding the modifier into the reaction kettle, vacuumizing, and reacting the modifier with the prepolymer to obtain a first clear solution;
adding the initiator into the first clarified solution, and stirring to obtain a second clarified solution;
pouring the second clarified solution into a mould, and heating and curing; and
and cooling and then removing the mold to obtain the X-ray-proof glass.
8. The method for producing an X-ray resistant glass according to claim 7, wherein the prepolymer is a mixture of methacrylic acid, methyl methacrylate and a lead-containing compound.
9. The method for preparing the X-ray resistant glass according to claim 8, wherein the lead-containing compound is one or more of basic lead carbonate, lead acetate trihydrate, lead acetate, lead nitrate, lead oxide, lead phosphate, lead sulfate, lead acetate and lead bromide; and/or the methacrylate is one or more of methyl methacrylate, ethyl methacrylate and propyl methacrylate.
10. The method of claim 7, wherein the modifier is one or more of 2-hydroxyethyl methacrylate, neopentyl glycol and boric acid; and/or the initiator is one or more of tert-butyl peroxyneodecanoate, dibutyl peroxydicarbonate, tert-butyl peroxy2-ethylhexanoate, tert-butyl peroxyacetate and 1,1,3, 3-tetramethyl butyl peroxypivalate.
CN201911318466.5A 2019-12-19 2019-12-19 Formula and preparation method of X-ray-proof glass Pending CN110964144A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113563533A (en) * 2021-08-24 2021-10-29 江苏铁锚玻璃股份有限公司 Formula and synthesis method of lead-containing acrylic sheet
CN113999345A (en) * 2021-11-30 2022-02-01 江苏铁锚玻璃股份有限公司 Formula and preparation method of spherical organic glass
CN114437281A (en) * 2022-03-01 2022-05-06 深圳市新涛控股有限公司 Preparation method of X-ray shielding type transparent PMMA casting plate

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN88100180A (en) * 1988-01-20 1988-08-03 北京市有机玻璃制品厂 X-ray-preventing ultraviolet ray synthetic glass and method for making
CN109053948A (en) * 2018-08-16 2018-12-21 天长市瑞慈有机玻璃有限公司 A kind of X-ray-preventing ultraviolet light lucite tube and preparation method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN88100180A (en) * 1988-01-20 1988-08-03 北京市有机玻璃制品厂 X-ray-preventing ultraviolet ray synthetic glass and method for making
CN109053948A (en) * 2018-08-16 2018-12-21 天长市瑞慈有机玻璃有限公司 A kind of X-ray-preventing ultraviolet light lucite tube and preparation method

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113563533A (en) * 2021-08-24 2021-10-29 江苏铁锚玻璃股份有限公司 Formula and synthesis method of lead-containing acrylic sheet
CN113999345A (en) * 2021-11-30 2022-02-01 江苏铁锚玻璃股份有限公司 Formula and preparation method of spherical organic glass
CN113999345B (en) * 2021-11-30 2023-08-29 江苏铁锚玻璃股份有限公司 Formula of spherical organic glass and preparation method thereof
CN114437281A (en) * 2022-03-01 2022-05-06 深圳市新涛控股有限公司 Preparation method of X-ray shielding type transparent PMMA casting plate
CN114437281B (en) * 2022-03-01 2023-11-07 深圳市新涛新材料股份有限公司 Preparation method of X-ray shielding transparent PMMA casting plate

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Application publication date: 20200407