WO2013155891A1 - 碳化硼高聚纤维 - Google Patents

碳化硼高聚纤维 Download PDF

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Publication number
WO2013155891A1
WO2013155891A1 PCT/CN2013/071485 CN2013071485W WO2013155891A1 WO 2013155891 A1 WO2013155891 A1 WO 2013155891A1 CN 2013071485 W CN2013071485 W CN 2013071485W WO 2013155891 A1 WO2013155891 A1 WO 2013155891A1
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Prior art keywords
boron carbide
parts
antioxidant
catalyst
polyethylene emulsion
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PCT/CN2013/071485
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English (en)
French (fr)
Inventor
夏华松
夏康凯
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Xia Huasong
Xia Kangkai
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Application filed by Xia Huasong, Xia Kangkai filed Critical Xia Huasong
Priority to KR20147032011A priority Critical patent/KR20140147892A/ko
Priority to EP13778425.2A priority patent/EP2840171B1/en
Priority to JP2015506081A priority patent/JP6140809B2/ja
Priority to US14/394,970 priority patent/US9187618B2/en
Publication of WO2013155891A1 publication Critical patent/WO2013155891A1/zh

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    • 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
    • C08K3/38—Boron-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62272—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
    • C04B35/62277—Fibres based on carbides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63408—Polyalkenes
    • 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
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
    • 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
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
    • C08K5/3432—Six-membered rings
    • C08K5/3437—Six-membered rings condensed with carbocyclic rings
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/08—Melt spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/04—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins
    • 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
    • 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
    • G21F3/00—Shielding characterised by its physical form, e.g. granules, or shape of the material
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3821—Boron carbides
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2101/00—Inorganic fibres
    • D10B2101/10—Inorganic fibres based on non-oxides other than metals
    • D10B2101/14—Carbides; Nitrides; Silicides; Borides
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2321/00—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D10B2321/02—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polyolefins
    • D10B2321/021—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polyolefins polyethylene

Definitions

  • the present invention relates to a high polyfluorene. Background technique
  • China is a big country in China, but it is not a strong country in chemical fiber. According to experts and relevant departments, China's high-performance special fiber production is only one percent of world production.
  • the three high-performance fibers in the world today are: carbon fiber, aramid, high molecular weight polymer fibers. Carbon fiber is still in the test and primary production stage, and the product can only be used in the field of wear-resistant fillers.
  • High-molecular-weight polymerized polymers in Europe and the United States are used in bulletproof armor, bulletproof helmets, bulletproof armor for military installations and equipment, aerospace and other military fields, and the development of high-performance fibers is a manifestation of a country's comprehensive strength. The important material basis, for this reason, it is particularly urgent to accelerate the development of China's high-performance special fiber production and application from the national interest.
  • the object of the present invention is to invent a novel special material boron carbide high polyfluorene.
  • boron carbide high polymer fiber After long-term development and repeated experiments, a new material of boron carbide high polymer fiber was invented.
  • the raw materials needed for the material were: boron carbide, high polyethylene emulsion, hydrochloric acid, antioxidant, catalyst.
  • the boron carbide high polymer fiber of the invention can be used for manufacturing high-end guns, marine rescue, fire fighting, bulletproof and anti-riot decoration, biochemical nuclear industry treatment, etc., and can be widely applied in civil, aerospace and military defense.
  • the invention has excellent high and low temperature resistance, superior acid and alkali resistance, excellent stretchability, abrasion resistance and impact resistance, and can be used for a long time under the standard atmospheric pressure 170 21 001 environment. It has excellent acid and acid resistance. It is continuously immersed in caustic soda for 30 days under normal temperature and pressure, and continuously immersed in hydrochloric acid solution for 30 days.
  • the material body has no essential change.
  • the material has excellent stretchability, wear resistance and impact resistance.
  • the ability to strike and UV resistance, the strength of the ⁇ Vie is ten times that of the same section of steel wire, the fiber density is low, and it can float on the water surface; the elongation at break is low, and it has a strong ability to absorb energy, so it has outstanding impact resistance. Sex. It is resistant to ultraviolet radiation, neutrons and gamma rays; it has a low dielectric constant and high electromagnetic wave transmission.
  • the invention can be widely used in civil, nuclear, aerospace and military defense
  • the prepared boron carbide high polymer fiber fills the blank of similar products in China. This material is recyclable and non-polluting. Concrete it*
  • the invention relates to a novel material of boron carbide high polymer fiber, which is prepared from the following raw materials by weight:
  • the boron carbide is selected from the group consisting of boron carbide-wl 4, -w20, w28, w40; the high polyethylene emulsion is selected from the group consisting of HA sof t 80, G_FN, 85 CD IT in a polyethylene emulsion.
  • One type boron carbide-wl 4, -w20, w28, w40;
  • the high polyethylene emulsion is selected from the group consisting of HA sof t 80, G_FN, 85 CD IT in a polyethylene emulsion.
  • the antioxidant is selected from the group consisting of diphenylamine, p-phenylenediamine and dihydroquinoline in an antioxidant.
  • the catalyst i is one of the catalysts trifluoromethanesulfonic anhydride.
  • the invention also provides a method for preparing a novel material of carbon-boron high-polymer fiber, which is produced by using the above-mentioned raw materials by weight, and comprises the following steps:

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • High Energy & Nuclear Physics (AREA)
  • General Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Nanotechnology (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Fibers (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Artificial Filaments (AREA)

Abstract

一种碳化硼高聚纤维材料。制作该材料所需要的组分和措施为：碳化硼50—60份，浓度40%—50%的高聚乙烯乳液150—193份，37%浓度盐酸116份，抗氧剂3—5份，催化剂7份，2500—2800°C高温高压熔炉，耐高温纺丝炉。制得的材料具有耐高低温性能，耐酸碱性能，伸展性、耐磨抗冲击能力及耐紫外线性能。可用于制造枪炮、海事救援器材、消防救火器材、防弹防爆装甲、生化核工业处理等用途，在民用、航空航天和军事国防上可广泛应用。本材料可回收利用，无污染。

Description

技术领域
本发明涉及一种高聚紆维。 背景技术
中国是化紆大国， 但不是化纤强国， 椐专家介绍和有关部门 统计， 中国的高性能特种纤维的产量仅为世界产量的百分之一。 当今世界三大高性能纤维是： 碳纤维、 芳纶、 高分子量聚合纤维。 碳纤维尚处在试验和初级生产阶段， 产品只能应用在耐磨填料等 领域。 欧美发达国家高分子量聚合紆维 70¾以上用于防弹衣、 防 弹头盔、 军用设施和设备的防弹装甲， 航空航天等军事领域， 而 高性能纤维的发展是一个国家综合实力的体现，是建设现代化 强 国的重要物资基础， 为此，从国家利益出发大力加速发展我国的 高性能特种纤维的生产与应用尤显迫切。
本发明 目的是发明一种新型专用材料碳化硼高聚紆维。
经长期的研制及反复实验， 发明一种新材料碳化硼高聚纤维， 制作该材料所需原料为： 碳化硼， 高聚乙烯乳液， 盐酸， 抗氧剂， 催化剂。
本发明碳化硼高聚纤维可用于制造高端枪炮， 海事救援、 消 防救火、 防弹防暴装曱、 生化核工业处理等用途， 在民用、 航空 航天和军事国防上可广泛应用。 本发明具有极好的耐高低温性能， 超强的耐酸碱性能， 优异的伸展性、 耐磨、 抗冲击能力等性能， 在标准大气压下 170 21 001环境内可长期使用。 它有超强的耐 酸緘性能， 常温常压下在烧碱溶液中连续浸泡 30天， 在盐酸溶液 中连续浸泡 30天， 材料本体没有本质改变； 本材料有优异的伸展 性、 耐磨， 抗沖击能力及耐紫外线等性能， 紆维比强度是同等截 面钢丝的十多倍， 纤维密度低， 可浮于水面； 断裂伸长低， 具有 很强的吸收能量的能力， 因而具有突出的抗冲击性。 可抗紫外线 辐射， 防中子和 γ射线； 材料的介电常数低、 电磁波透射率高。
因此， 本发明可在民用、 核工业、 航空航天和军事国防上广 泛应用， 所制得的碳化硼高聚纤维填补了国内同类产品的空白。 本材料可回收利用， 无污染。 具体实 it*方式
本发明一种新型材料碳化硼高聚纤维， 由以下重量份的原料 制备而成：
碳化硼 50 60份
质量浓度 40¾ 50¾的高聚乙烯乳液 150-193份
质量浓度 37%的盐酸 116份
抗氧剂 3 5份
催化剂 Ί份
所述的碳化硼选自碳化硼 - wl 4、 - w20、 w28、 w40中的 - 种； 所述的高聚乙烯乳液选自聚乙烯乳液中的 HA sof t 80、 G_FN、 85 CD I T中的一种；
所述的抗氧剂选自抗氧剂中的二苯胺，对苯二胺和二氢喹啉等
' 所述^催化剂 i 自催化剂三氟甲基磺酸酐中的一种。
本发明还提出一种新型材料碳硼高聚纤维的制作方法，使用上 述重量份的原料制作， 包括以下步骤：
(1)将碳化堋泡入盐酸中 90 120分钟去除杂质；
(2)将除净烘千后的碳化硼放入 2600 °C的高温高压熔炉中融 化； 所得碳化硼熔融液体在耐高温纺丝炉内制得碳化硼原丝。
(3)在含抗氧剂的高聚乙烯乳液中， 加入催化剂， 将碳化硼原 丝放入， 在 15-30 个大气压作用下， 制得无机高分子聚合物， 即 碳化硼高聚纤维的初步产物。 初步产物通过氢氧化钙溶液进行表 面处理， 除净烘千后最终得到本碳化硼高聚纤维。

Claims

1、 一种碳化硼高聚纤维， 制作该材料所需原料为： 碳化硼， 高聚乙烯乳液， 盐酸， 抗氧剂， 催化剂。
2、 根据权利要求 1 所述的碳化硼高聚纤维， 制作该材料所需 原料的重量份为：
碳化硼 50 60份，
浓度 40¾ 50¾的高聚乙烯乳液 150-1 93份，
浓度 37%的盐酸 1 16份，
抗氧剂 3 5份，
催化剂 7份。
3、 根据权利要求 i或 2所述的专用材料， 所述的碳化硼选自碳化 硼 wl 4、 w20 , w28 , w40中的一种。
4、 根据权利要求 1或 2所述的专用材料， 所述的高聚乙烯乳液选 自聚乙烯乳液中的 HA- sof t 80、 GFN、 85-CDI T中的一种。
5、 根据权剩要求 1或 2所述的专用材料， 所述的抗氧剂选自抗氧 剂中的二苯胺， 对苯二胺和二氢喹淋等化合物及其衍生物或聚合 物中的任意一种。
6、 根据权剩要求 1或 2所述的专用材料， 所述的催化剂选自催化 剂三氟甲基磺酸酐中的一种。
7、 一种新型材料碳硼高聚纤维及制作方法包括以下步驟：
(1)将碳化硼泡入盐酸中 90 1 20分钟去除杂质；
(2)将除净烘千后的碳化硼放入 25 00 28001的高温高压熔炉中 融化； 所得碳化硼熔融液体在耐高温纺丝炉内制得碳化硼原丝；
(3)在含抗氧剂的高聚乙烯乳液中， 加入催化剂， 将碳化硼原丝 放入， 在 1 5-30 个大气压作用下， 制得无机高分子聚合物， 即碳 化硼高聚纾维的初步产物； 初步产物通过氢氧化钙溶液进行表面 处理， 除净烘千后最终得到本碳化硼高聚纤维。
PCT/CN2013/071485 2012-04-16 2013-02-07 碳化硼高聚纤维 WO2013155891A1 (zh)

Priority Applications (4)

Application Number Priority Date Filing Date Title
KR20147032011A KR20140147892A (ko) 2012-04-16 2013-02-07 탄화붕소의 고분자 섬유
EP13778425.2A EP2840171B1 (en) 2012-04-16 2013-02-07 Method of fabricating a highly polymeric fiber of boron carbide
JP2015506081A JP6140809B2 (ja) 2012-04-16 2013-02-07 炭化ホウ素高重合ポリマー繊維
US14/394,970 US9187618B2 (en) 2012-04-16 2013-02-07 Boron carbide high polymeric fiber

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CN201210108701.8 2012-04-16
CN2012101087018A CN102644131B (zh) 2012-04-16 2012-04-16 碳化硼高聚纤维

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CN104591737A (zh) * 2014-12-31 2015-05-06 东莞市高能磁电技术有限公司 碳化硼材料及其制造方法
CN107160789A (zh) * 2017-04-06 2017-09-15 江阴中达软塑新材料股份有限公司 一种药用包装专用薄膜
KR20200019070A (ko) 2018-08-13 2020-02-21 에스케이씨솔믹스 주식회사 탄화붕소 소결체의 제조방법 및 성형다이

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US9187618B2 (en) 2015-11-17
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EP2840171B1 (en) 2017-09-27
JP6140809B2 (ja) 2017-05-31
US20150126649A1 (en) 2015-05-07
JP2015517037A (ja) 2015-06-18
EP2840171A1 (en) 2015-02-25
CN102644131A (zh) 2012-08-22
EP2840171A4 (en) 2015-12-23

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