阅读说明：本技术 一种防护中子辐射纤维材料的工业生产方法 (Industrial production method of neutron radiation protection fiber materials ) 是由 刘小秦 于 2019-09-03 设计创作，主要内容包括：一种防护中子辐射纤维材料的工业生产方法涉及防护中子辐射纤维材料的生产方法。主要是为解决现有的防护中子辐射纤维材料存在防中子能力较弱,纤维强度不足的问题而发明的。将原料尼龙-6切片和富集硼-10碳化硼、抗氧剂1010一起加入到混合釜,混合均匀后进入螺杆挤压机熔融挤出,从喷丝板纺丝,经气流冷却牵伸,卷绕,经管纱、络筒、并线、捻线得到共混熔纺原丝纤维,共混熔纺原丝纤维与碳纤维互捻合股,然后经络筒、整经、穿经结,形成经线。纬纱采用与经线相同的共混熔纺原丝纤维。经线、纬线通过织布机,织造出可防中子、X射线辐射的高性能机织布料。优点是具有很强的中子吸收能力,强度高。(an industrial production method of neutron radiation protection fiber material relates to a production method of neutron radiation protection fiber material, which is invented mainly for solving the problems of weak neutron radiation protection capability and insufficient fiber strength of the existing neutron radiation protection fiber material, the raw material nylon-6 slice, boron-10-enriched carbide and antioxidant 1010 are added into a mixing kettle, are uniformly mixed and then enter a screw extruder to be melted and extruded, and then are spun from a spinneret plate, cooled and drafted by air flow, wound, and then are subjected to tube spinning, winding, doubling and twisting to obtain the blending melt-spun precursor fiber, the blending melt-spun precursor fiber and the carbon fiber are twisted and plied with each other, and then are subjected to winding, warping and warp-threading to form warp yarns.)

1, an industrial production method of neutron radiation protection fiber material, which is characterized in that:

, adding raw materials of nylon-6 slices, boron-10-enriched boron carbide and an antioxidant into a mixing kettle, uniformly mixing, then putting into a screw extruder for melt extrusion, metering by a metering pump, spinning from a spinneret plate, cooling and drafting by air flow, winding, obtaining blended melt-spun precursor fibers by cop, spooling, doubling and twisting, twisting the blended melt-spun precursor fibers and carbon fibers for stranding, and then spooling, warping and tying to form warps;

secondly, adding the raw material nylon-6 slices, boron-10-enriched boron carbide and an antioxidant into a mixing kettle, uniformly mixing, then feeding into a screw extruder for melt extrusion, metering by a metering pump, spinning from a spinneret plate, cooling and drafting by airflow, winding, and then feeding into the processes of doubling, twisting and weft winding to form weft;

and thirdly, weaving the warps and the wefts through a loom to obtain the high-performance woven fabric capable of preventing neutron and X-ray radiation.

2. The industrial production method of a neutron radiation protection fiber material according to claim 1, wherein: the enriched boron-10 boron carbide: (¹⁰B₄C) The abundance ratio of boron-10 is above 96, and the particle size distribution is 0.5-40 microns.

3. The industrial production method of a neutron radiation protection fiber material according to claim 1, wherein: added of¹⁰B₄The weight ratio of the C to the nylon-6 chips is 30-35: 100.

4. The industrial production method of a neutron radiation protection fiber material according to claim 1, wherein: the weight ratio of the antioxidant to the nylon-6 slice is 0.1-0.5: 100.

5. the industrial production method of a neutron radiation protection fiber material according to claim 1, wherein: the warp is produced by plying and twisting 1 blended melt-spun precursor fiber with 1 carbon fiber.

The technical field is as follows:

the invention relates to a production method of fiber materials for protecting neutron radiation.

The application of nuclear science and technology has been deepened into various fields of nuclear powered ships, aerospace, medical radiology, food processing, nondestructive testing, nuclear engineering, agriculture, biomedicine and the like which concern national safety and national civilization and become indispensable components of modern society, X rays, gamma rays, neutron rays and the like generated by nuclear radiation not only can cause new environmental pollution (nuclear pollution) but also can seriously harm the health and safety of human bodies, and in high-energy rays of nuclear radiation, the harm of the neutron rays is the greatest, so the protection of the neutron rays is very important.

The application shows that the traditional single neutron shielding structure material has many disadvantages and is difficult to meet the protection requirement of a special structure, the selection of the polymer and the neutron absorber can directly influence the shielding performance of the protective material, the thermal neutron absorption cross section of boron-10 is 3837 targets, which is more than 50 times of that of the concrete neutron protective material, the protective material containing boron-10 usually exists in the form of boron, borate or boron carbide, and because of the high boron content, excellent physical and chemical properties of boron carbide, radioactive isotopes generated in the middle of the application engineering, the secondary ray energy is low, the boron resource is rich, the boron carbide waste is easy to treat, so the boron carbide is widely used as the nuclear neutron protective material.

Research and application show that lead as a neutron shielding material is toxic and high in density, mainly protects gamma rays and has a less ideal neutron shielding effect; the concrete protective material occupies a larger space and is not easy to move in the using process; boron-aluminum alloy and boron steel can improve the protective performance by increasing the boron content, but also can reduce the structural strength of the composite material. The chromium rod has excellent ray absorption performance and mechanical performance, but the chromium rod is high in price and can generate secondary rays.

kinds of paint which uses 793 resin as curing agent and can shield and absorb neutron radiation is prepared by Huangyi ping et al, but the toughness is not good, so that the special structure protection requirement can not be met.

kinds of B's are made up by Chaihao et al₄The C/SEBS neutron shielding composite material has the comprehensive performance of .

Studies have shown that polyethylene materials are easily softened and melted at high temperatures and are highly likely to have severe neutron leak incidents. The flexible polyethylene protective material can release secondary gamma rays after capturing thermal neutrons, so that the capability of absorbing the thermal neutrons is reduced to a great extent, the temperature application range is narrow, the service life is short, and the replacement frequency is high.

The boron/polymethyl methacrylate composite material has strong neutron shielding capability, but short service life. The boron carbide/phenolic resin composite material needs a considerable thickness to meet the protection requirement, and the application range of the material is limited.

In the polypropylene/boron carbide blending system of Wangchun scholar and the like, 40% of boron carbide micro powder is added, the using amount of titanate as an auxiliary agent is 1.5-2.5%, the core material blending is subjected to composite spinning, the breaking strength of the obtained fiber is 2.06cN/dtex, the breaking elongation is 37%, the hot melting temperature is 163 ℃, and the non-woven fabric prepared from the fiber has -determined shielding effect on neutrons.

The domestic patent adopts the blending of boron, heavy metal compound and polypropylene, and then melt spinning to prepare the core-sheath type anti-neutron and X-ray fiber with the boron carbide content of 35 percent. The fiber strength is 2327cN/tex, the breaking elongation is 20-40%, and the fiber is processed into knitted fabric, woven fabric and non-woven fabric for the periphery of an atomic energy reactor, so that the neutron radiation protection shielding rate can reach more than 44%. But also has the problems of low neutron radiation protection shielding rate, insufficient fiber strength and low temperature resistance.

The invention content is as follows:

the invention aims to solve the technical problem of providing industrial production methods of fiber materials capable of protecting neutron radiation, which have strong neutron absorption capacity and high neutron radiation protection shielding rate.

The above object is achieved by: the boron-10-enriched boron carbide, nylon-6 slices and an antioxidant are blended and melt-spun to prepare 100dtex-200 dtex protofilament fiber with the boron carbide content of 30% -35% (the boron-10 content is 23.07% -26.92%). The blended melt-spun precursor fiber and MH300-3K carbon fiber are stranded and twisted with each other to form warp, the blended melt-spun precursor fiber is doubled and twisted to form weft, and the warp and the weft are woven to form the high-performance cloth capable of protecting against neutron and X-ray radiation.

The specific method comprises the following steps:

, slicing nylon-6 (PA-6) and carbonizing the enriched boron-10Boron (C)¹⁰B₄C) Adding the antioxidant 1010 into a mixing kettle, uniformly mixing, then feeding into a screw extruder for melt extrusion, metering by a metering pump, spinning from a spinneret plate, cooling and drafting by air flow, winding by cop, spooling, doubling, twisting to obtain blended melt-spun precursor fibers, mutually twisting and stranding the blended melt-spun precursor fibers and carbon fibers, and then spooling, warping, and tying to form warps.

Secondly, the weft adopts blended melt-spun raw silk fibers the same as the warp, namely raw material nylon-6 (PA-6) is sliced and boron-10 boron carbide (B) is enriched¹⁰B₄C) Adding the antioxidant 1010 into a mixing kettle, uniformly mixing, then feeding into a screw extruder for melt extrusion, metering by a metering pump, spinning from a spinneret plate, cooling and drafting by airflow, winding, and then feeding into the processes of doubling, twisting and winding to form weft.

And thirdly, weaving the warps and the wefts through a loom to obtain the high-performance woven fabric capable of preventing neutron and X-ray radiation.

The nylon-6 chip is a conventional industrial product purchased from the market, has the relative viscosity of 1.7686 η r/dl/g and the melting temperature of 221.7 ℃, and is enriched with boron-10 boron carbide (B)¹⁰B₄C) Boron-10 abundance of over 96, particle size distribution of 0.5-40 microns, added¹⁰B₄The weight ratio of C to nylon-6 is as follows:

¹⁰B₄c: nylon-6 = 30-35: 100;

the antioxidant 1010 is high molecular weight hindered phenol antioxidants with chemical name of [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (molecular formula: C)₇₃H₁₀₈O₁₂) The weight ratio of the antioxidant to the nylon-6 slice is as follows:

antioxidant: nylon-6 chip = 0.1-0.5: 100, respectively;

the mixing kettle is a stainless steel container with stirring.

The middle temperature of the screw extruder is 600-610 ℃, and the tail temperature is 585-595 ℃. The specification of the protofilament spun by the spinneret plate is 100dtex-200 dtex.

The blended melt-spun precursor fiber and the carbon fiber are twisted with each other during the production of the warp, so as to increase the strength of the warp, namely 1 blended melt-spun precursor fiber is twisted with each other corresponding to 1 carbon fiber.

The carbon fiber is made of MH300-3K brand, the tensile strength is more than or equal to 3500MPa, the elongation at break is more than or equal to 1.5 percent, and the linear density is 198 +/-2 g/1000 m.

The weft is different from the warp in that the weft is directly formed by blending melt-spun precursor fibers and is not doped with carbon fibers.

The cloth woven by the warps and the wefts has a boron-10 content of 23.07-26.92%, has strong neutron absorption capacity, is processed into knitted fabrics or woven fabrics with the thickness of 0.4 mm-0.6 mm and is used around an atomic energy reactor, the neutron radiation protection shielding rate can reach 98.5-99.5%, and the neutron quantity is lower than the environmental level; carrying out high-speed transformation on the fabric according to the following steps of carrying out; the paint has excellent flexibility, and the Shore hardness is 6.5HD-7.0 HD; the breaking strength of the fiber is 7.26cN/dtex-7.83 cN/dtex; the exercise elongation is 40-42%, and the hot melting temperature is 343-347 ℃.

The invention has the advantages that: the enriched boron-10 boron carbide, nylon-6 slices and antioxidant 1010 are blended and melt-spun to prepare 100dtex-200 dtex protofilament fiber with the boron carbide content of 30-35 percent (the boron-10 content is 23.07-26.92 percent). The 100dtex-200 dtex protofilament fiber and the domestic MH300-3K carbon fiber are stranded and twisted to form a warp, the 100dtex-200 dtex protofilament fiber is doubled and twisted to form a weft, and the warp and the weft are woven to form the high-performance cloth. The cloth has strong neutron absorption capacity, is processed into knitted fabric or woven fabric with the thickness of 0.4-0.6 mm and is used for the periphery of an atomic energy reactor, the neutron radiation protection shielding rate can reach 98.5-99.5%, and the neutron quantity is lower than the environmental level; the high-flexibility polyurethane composite material has excellent flexibility, the Shore hardness is 6.5HD-7.0HD, the cutting performance is excellent, and the high-flexibility polyurethane composite material can be used for producing various protective clothing and covers; carrying out high-speed cultivation on the fabric with the density of 1.25/cm-1.29/cm, wherein the low density facilitates movement, and the breaking strength of the fiber is 7.26cN/dtex-7.83 cN/dtex; the exercise elongation is 40-42%, the hot melting temperature is 343-347 ℃, the thermal property is excellent, and the protection requirement of a special structure can be met.

The specific implementation mode is as follows:

the boron-10-enriched boron carbide, nylon-6 slices and an antioxidant are blended and melt-spun to prepare 100dtex-200 dtex protofilament fiber with the boron carbide content of 30% -35% (the boron-10 content is 23.07% -26.92%). The blended melt-spun precursor fiber and MH300-3K carbon fiber are stranded and twisted with each other to form warp, the blended melt-spun precursor fiber is doubled and twisted to form weft, and the warp and the weft are woven to form the high-performance cloth capable of protecting against neutron and X-ray radiation.

The specific method comprises the following steps:

, slicing nylon-6 (PA-6) and enriching boron-10 boron carbide¹⁰B₄C) Adding the antioxidant 1010 into a mixing kettle, uniformly mixing, then feeding into a screw extruder for melt extrusion, metering by a metering pump, spinning from a spinneret plate, cooling and drafting by air flow, winding by cop, spooling, doubling, twisting to obtain blended melt-spun precursor fibers, mutually twisting and stranding the blended melt-spun precursor fibers and carbon fibers, and then spooling, warping, and tying to form warps.

Secondly, the weft adopts blended melt-spun raw silk fibers the same as the warp, namely raw material nylon-6 (PA-6) is sliced and boron-10 boron carbide (B) is enriched¹⁰B₄C) Adding the antioxidant 1010 into a mixing kettle, uniformly mixing, then feeding into a screw extruder for melt extrusion, metering by a metering pump, spinning from a spinneret plate, cooling and drafting by airflow, winding, and then feeding into the processes of doubling, twisting and winding to form weft.

And thirdly, weaving the warps and the wefts through a loom to obtain the high-performance woven fabric capable of preventing neutron and X-ray radiation.

The nylon-6 chip is a conventional industrial product purchased from the market, has the relative viscosity of 1.7686 η r/dl/g and the melting temperature of 221.7 ℃, and is enriched with boron-10 boron carbide (B)¹⁰B₄C) Boron-10 abundance of over 96, particle size distribution of 0.5-40 microns, added¹⁰B₄The weight ratio of the C to the nylon-6 slices is as follows:

¹⁰B₄c: nylon-6 chip = 30-35: 100;

the antioxidant 1010 is high molecular weight hindered phenol antioxidantsThe oxygen agent has the chemical name of [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (molecular formula: C)₇₃H₁₀₈O₁₂) The weight ratio of the antioxidant to the nylon-6 slice is as follows:

antioxidant: nylon-6 chip = 0.1-0.5: 100, respectively;

the mixing kettle is a stainless steel container with stirring.

The middle temperature of the screw extruder is 600-610 ℃, and the tail temperature is 585-595 ℃. The specification of the protofilament spun by the spinneret plate is 100dtex-200 dtex.

The blended melt-spun precursor fiber and the carbon fiber are twisted with each other during the production of the warp, so as to increase the strength of the warp, namely 1 blended melt-spun precursor fiber is twisted with each other corresponding to 1 carbon fiber.

The carbon fiber is made of MH300-3K brand, the tensile strength is more than or equal to 3500MPa, the elongation at break is more than or equal to 1.5 percent, and the linear density is 198 +/-2 g/1000 m.

The weft is different from the warp in that the weft is directly formed by blending melt-spun precursor fibers and is not doped with carbon fibers.

The cloth woven by the warps and the wefts has the boron-10 content of 23.07-26.92%, has strong neutron absorption capacity, is processed into knitted fabric or woven fabric with the thickness of 0.4-0.6 mm and is used for the periphery of an atomic energy reactor, the neutron radiation protection shielding rate can reach 98.5-99.5%, and the neutron quantity is lower than the environmental level; carrying out high-speed transformation on the fabric according to the following steps of carrying out; the paint has excellent flexibility, and the Shore hardness is 6.5HD-7.0 HD; the breaking strength of the fiber is 7.26cN/dtex-7.83 cN/dtex; the exercise elongation is 40-42%, and the hot melting temperature is 343-347 ℃.