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Carborane-containing organic matter and neutron radiation protection material polyester and its preparation

A technology of carborane and organic matter, applied in the fields of compounds containing elements of group 3/13 of the periodic table, organic chemistry, single-component polyester artificial filament, etc. Silk equipment and process complex, poor durability and fastness, etc., to achieve the effect of not easy to wash or rub off, high boron content, good heat resistance

Active Publication Date: 2017-08-15
BEIHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first method is because neutron absorbers such as boron compounds are protected by skin polymers and are not easy to fall off, but the spinning equipment and process are complicated, the investment is large, and the boron content is not high enough.
In the second and third methods, since the neutron absorber and the fiber are non-chemically bonded and are on the surface of the fiber, it is easy to fall off due to washing and friction, and the durability and fastness are poor.
As we all know, the number-average molecular weight of polyester with fiber-forming properties is at least 10,000, so it is difficult to prepare neutron radiation-resistant fibers

Method used

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  • Carborane-containing organic matter and neutron radiation protection material polyester and its preparation
  • Carborane-containing organic matter and neutron radiation protection material polyester and its preparation
  • Carborane-containing organic matter and neutron radiation protection material polyester and its preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] The preparation method of embodiment 1 5-(o-carborane-1'-methyleneoxy) dimethyl isophthalate (BDMI)

[0058] The route is as follows:

[0059]

[0060] In a three-necked flask, add 0.22mol 5-hydroxyisophthalic acid, 300ml methanol and 12ml concentrated sulfuric acid in sequence, and react under reflux in an oil bath at 70°C, monitor by TLC, and cool to room temperature naturally after the reaction. The reaction solution was slowly added to distilled water, and a large amount of white precipitates precipitated out. They were suction filtered and vacuum-dried to obtain a white powder with a yield of 96.8%. The product was methyl 5-hydroxyisophthalate with a melting point of 169°C.

[0061] In the three-necked flask, 0.22mol dimethyl 5-hydroxyisophthalate, 0.48mol anhydrous potassium carbonate and solvent DMF were added in sequence. Oil bath at 60°C, stirred for 1 hour, cooled to room temperature, slowly added dropwise 0.24mol 3-bromopropyne, kept at 25°C for reaction,...

Embodiment 2

[0064] The boron-containing organic hybrid polyester B-PET synthetic method adopts the transesterification method, and the specific steps include:

[0065] A. by the proportioning amount of table 1, dimethyl terephthalate, ethylene glycol, 5-(ortho-carborane-1 '-methyleneoxy) dimethyl isophthalate (embodiment 1 made), and catalyzer zinc acetate 0.01g is dropped in the reactor of 1L, logical nitrogen protection, heat up;

[0066] B. After heating up to 190°C, start stirring, control the temperature at 185°C-190°C, and react for 3 hours;

[0067] C. Raise the temperature to 280°C, stop nitrogen flow, vacuumize, and keep for 30 minutes;

[0068] D. Vacuumize to 133Pa, keep warm at 280℃~285℃, and react for 3h;

[0069] E. Stop the reaction, feed nitrogen gas under normal pressure, open the reaction kettle, slowly pour the polyester melt into distilled water to discharge while hot, and dry in vacuum to obtain boron-containing organic hybrid polyester B-PET.

[0070] F. Cut boron...

Embodiment 3-5

[0072] The operation steps are the same as in Example 1, except that the ratio of raw materials is different. The products prepared in Examples 2-5 are marked as B-PET-1, B-PET-2, B-PET-3, and B-PET-4. The ratio of raw materials is shown in Table 1.

[0073] Table 1 Synthesis of boron-containing organic hybrid polyester (B-PET) raw material components and mass ratio

[0074]

[0075] The physical and chemical properties and tensile strength tests of the spun fibers were carried out. See Table 2 and Table 3 for the performance data of boron-containing organic hybrid polyester B-PET. For the tensile stress-strain relationship of fiber monofilament, see figure 1. As a comparison, the corresponding parameters of polyester polyester (PET) were tested.

[0076] Table 2 Properties of boron-containing organic hybrid polyester B-PET

[0077]

[0078]

[0079] It can be determined from the intrinsic viscosity and molecular weight that the values ​​of n and m in the molecu...

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Abstract

The invention provides a carborane-containing organic matter, namely, 5-(o-carborane-1'-methyleneoxy) dimethyl isophthalate, as well as a neutron radiation protection material prepared from the compound. The material is PET (polyethylene terephthalate), a structural formula of the material is represented in the specification, wherein n is in a range from 1 to 200, m is in a range from 1 to 200, and k is in a range from 1 to 6. The carborane structure is introduced into a main chain lateral group structure of PET through chemical bonds, monomers with different k values and boric dicarboxylic acid structures are selected and a polymerization process is adopted to control n and m, so that polymer PET chips with different boron content and fiber forming features are obtained, and with adoption of direct melt spinning, organic hybrid PET fibers with different mechanical properties, different thermal properties and different boron content are obtained.

Description

technical field [0001] The invention belongs to the field of materials, and in particular relates to a neutron radiation-resistant polymer material and a synthesis method thereof. Background technique [0002] Neutrons have strong penetrating power, and the damage to the human body is far greater than that of the same dose of X and γ-rays, which seriously damage the human stomach and male glands, and induce tumor formation. In terms of national defense, neutron weapons are the third-generation nuclear weapons that have been deployed in the world. After the explosion, they will cause great harm to military personnel, such as the drivers and passengers of tanks and chariots, chemical defense soldiers and medical personnel entering the scene. Protect against neutron radiation. In civilian fields, such as nuclear reactors, accelerators, magnetic confinement fusion Tokamak devices, operation and maintenance of nuclear powered ships, geological exploration, oil well detection, ne...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/02C08G63/698D01F6/62
CPCC07F5/05C08G63/6986D01F6/62
Inventor 陈功胡建景冯晨蔡益波
Owner BEIHANG UNIV
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