WO2020244523A1 - 一种尼龙粉末的制备方法及应用 - Google Patents

一种尼龙粉末的制备方法及应用 Download PDF

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WO2020244523A1
WO2020244523A1 PCT/CN2020/094029 CN2020094029W WO2020244523A1 WO 2020244523 A1 WO2020244523 A1 WO 2020244523A1 CN 2020094029 W CN2020094029 W CN 2020094029W WO 2020244523 A1 WO2020244523 A1 WO 2020244523A1
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nylon powder
nylon
acid
mass
antioxidant
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PCT/CN2020/094029
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English (en)
French (fr)
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韩冰
黄玉安
杨少锋
王新迪
章峻
莫宏
陈汝建
曹潇
李书航
曹沈炀
徐阳
韩东苏
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南京工程学院
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Publication of WO2020244523A1 publication Critical patent/WO2020244523A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/36—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino acids, polyamines and polycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
    • C08G69/265—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids from at least two different diamines or at least two different dicarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers

Definitions

  • the invention belongs to the technical field of nylon materials, and particularly relates to a preparation method and application of nylon powder.
  • the encapsulated buckle for underwear uses nylon encapsulation. It has the characteristics of non-toxic, anti-rust, salt spray resistance, beautiful coating, easy to dye, and high color fastness. It is widely used in the field of underwear encapsulated buckle. At present, mainly foreign nylon 11, and domestic nylon powders prepared from nylon 1010 and nylon 1012 are used in this field, but the cost is relatively high, which is not conducive to promotion.
  • This application mainly proposes a preparation method and application of nylon powder, which solves the technical problems of high cost in the prior art and is not conducive to popularization. It has the advantages of easy availability of raw materials, low cost, excellent performance, and convenience. Preparation characteristics.
  • a preparation method of nylon powder includes the following steps:
  • the second step Add 2.1-7.5% of the total mass of the raw materials to the raw materials, and mix them evenly to obtain a mixture;
  • the third step Put the mixture into the high pressure reactor, seal, replace with nitrogen, discharge the air in the kettle, fill with nitrogen to 0.05-0.2MPa, and increase the temperature.
  • the temperature of the material rises to 200°C and the pressure reaches 1.2MPa, the temperature and pressure will start , Time 2 hours;
  • the fourth step then evenly release the pressure to normal pressure within 2 hours, and keep it at normal pressure for 2 hours;
  • the fifth step Fill nitrogen to 0.2MPa, open the discharge valve, the material is pelletized by the injection lead, cold water tank, pelletizer, and vacuum dried to obtain nylon resin;
  • the sixth step the nylon resin is made into nylon powder by mechanical powdering or chemical powdering.
  • the additives in the second step are antioxidants, brighteners, surface treatment agents and molecular weight regulators.
  • the brightener is a compound brightener
  • the surface treatment agent is one or more complexes of anionic surfactants, such as sodium dodecylbenzene sulfonate,
  • anionic surfactants such as sodium dodecylbenzene sulfonate
  • the molecular weight regulator is adipic acid, and the added amount is 0.1-0.5% of the total mass of the mixture.
  • the mixing speed in the second step is 1000-2000r/min
  • the mixing time is 2-5min
  • the pressure relief speed in the fourth step is 0.02-0.12MPa/min
  • the fifth step Dry under medium vacuum to moisture content ⁇ 0.5%.
  • the mechanical powdering step in the sixth step is to add nylon resin with 1% by mass of antioxidant 1010 and 10% by mass of titanium dioxide, and then modify it by an extruder. After drying, the nylon powder is obtained by cryogenic crushing and powder screening.
  • the chemical powdering step in the sixth step is to put nylon resin into an autoclave, add 1% by mass of antioxidant 1010 and 10% by mass of titanium dioxide, and add 96 % Ethanol, the weight of the ethanol is 3-4 times the weight of the nylon resin, dissolving at 170-180°C, cooling and precipitation, centrifugal separation, drying, and sieving to obtain nylon powder.
  • the present invention also provides the application of the nylon powder prepared by the nylon powder preparation method in the preparation of nylon encapsulated buttons.
  • the product has a melting point of 172 ⁇ 190°C, a melt index (230°C, 2.16kg): 40-56g/10 minutes, hardness (Shore hardness): 68-70, toughness: the spline is continuously folded in half.
  • Coating color bright color, no white spots, no color spots, high gloss, smooth surface.
  • the color of the rubber buckle has no obvious change in outdoor sunshine for 30 days.
  • a preparation method of nylon powder includes the following steps:
  • Step 1 Weigh 87 kg of hexamethylene diamine, 153 kg of sebacic acid, 60 kg of caprolactam, 4.5 kg of antioxidant, 1.5 kg of brightener, and 1 kg of sodium dodecyl benzene sulfonate according to the mass ratio. 600 grams of adipic acid, the antioxidant is made up of 500 grams of phosphorous acid, 2 kilograms of antioxidant 1098, and 2 kilograms of antioxidant 168.
  • the brightener is composed of 500 grams of calcium stearate, poly A compound of 500 grams of ether modified water-soluble silicone oil and 500 grams of benzoin;
  • Step 2 Mix the mixture evenly, the mixing speed is 1000-2000r/min, and the mixing time is 2-5min;
  • the third step Put the mixture into the autoclave, seal, replace with nitrogen, discharge the air in the kettle, fill with nitrogen to 0.2MPa, and increase the temperature. When the temperature of the material rises to 200°C and the pressure reaches 1.2MPa, the temperature and pressure will be maintained. 2 hours;
  • the fourth step then evenly release the pressure to normal pressure within 2 hours, at a pressure release rate of 0.1 MPa/min, and keep it at normal pressure for 2 hours;
  • Step 5 Fill with nitrogen to 0.2MPa, open the discharge valve, pellet the material through the injection lead, cold water tank, pelletizer, and vacuum dry to a moisture content ⁇ 0.5% to obtain nylon resin.
  • Toughness The spline is constantly folded in half.
  • the sixth step adding nylon resin to 1% by mass of antioxidant 1010 and 10% by mass of titanium dioxide, modified by an extruder, dried, and then crushed and sieved to obtain nylon powder;
  • Step 7 Prepare nylon encapsulated buckles from nylon powder. First prepare encapsulated buckle embryos, then heat the embryos into the vibrating plate, and powder the embryos. The powdered embryos are heated by a heating belt and calendered to obtain a nylon bag. The plastic buttons are dyed in an acid dye with a concentration of 1% at 80°C for 20 minutes, and then washed with water.
  • Coating color The color is gorgeous, no white spots, no stains, high gloss, smooth surface; outdoor sunshine for 30 days, no obvious change in color.
  • a preparation method of nylon powder includes the following steps:
  • Step 1 Weigh 90 kg of hexamethylene diamine, 180 kg of dodecanedioic acid, 30 kg of caprolactam, 3.5 kg of antioxidant, 2 kg of brightener, and 0.5 of sodium dodecyl benzene sulfonate according to the mass ratio.
  • Kilograms 800 grams of adipic acid
  • the antioxidant is made up of 500 grams of phosphorous acid, 1098 2 kilograms of antioxidants, and 168 1 kilograms of antioxidants.
  • the brightener is 500 grams of calcium stearate, poly A compound of 1000 grams of ether-modified water-soluble silicone oil and 500 grams of benzoin;
  • Step 2 Mix the mixture evenly, the mixing speed is 1000-2000r/min, and the mixing time is 2-5min;
  • the third step Put the mixture into the autoclave, seal, replace with nitrogen, discharge the air in the kettle, fill with nitrogen to 0.2MPa, and increase the temperature. When the temperature of the material rises to 200°C and the pressure reaches 1.2MPa, the temperature and pressure will be maintained. 2 hours;
  • the fourth step then evenly release the pressure to normal pressure within 2 hours, at a pressure release rate of 0.1 MPa/min, and keep it at normal pressure for 2 hours;
  • Step 5 Fill with nitrogen to 0.2MPa, open the discharge valve, pellet the material through the injection lead, cold water tank, pelletizer, and vacuum dry to a moisture content ⁇ 0.5% to obtain nylon resin.
  • Toughness The spline is constantly folded in half.
  • Step 6 Put the nylon resin into the autoclave, add 1% by mass of antioxidant 1010 and 10% by mass, and put in 96% ethanol.
  • the weight of the ethanol is 3-4 times the weight of the nylon resin. Dissolve at a high temperature of 170-180°C, precipitate out after cooling down, centrifuge, dry, and sieve to obtain nylon powder;
  • Step 7 Prepare nylon encapsulated buckles from nylon powder. First prepare encapsulated buckle embryos, then heat the embryos into the vibrating plate, and powder the embryos. The powdered embryos are heated by a heating belt and calendered to obtain a nylon bag. The plastic buttons are dyed in acid dye with a concentration of 2% at 70°C for 20 minutes, and then washed with water.
  • Coating color The color is gorgeous, no white spots, no stains, high gloss, smooth surface; outdoor sunshine for 30 days, no obvious change in color.
  • a preparation method of nylon powder includes the following steps:
  • the first step Weigh 114 kilograms of hexamethylene diamine, 144 kilograms of sebacic acid, 42 kilograms of adipic acid, 3 kilograms of antioxidant, 1.5 kilograms of brightener, and 1.5 kilograms of sodium dodecyl benzene sulfonate according to the mass ratio.
  • the brightener is 500 grams of calcium stearate, poly A compound of 500 grams of ether modified water-soluble silicone oil and 500 grams of benzoin;
  • Step 2 Mix the mixture evenly, the mixing speed is 1000-2000r/min, and the mixing time is 2-5min;
  • the third step Put the mixture into the autoclave, seal, replace with nitrogen, discharge the air in the kettle, fill with nitrogen to 0.2MPa, and increase the temperature. When the temperature of the material rises to 200°C and the pressure reaches 1.2MPa, the temperature and pressure will be maintained. 2 hours;
  • the fourth step then evenly release the pressure to normal pressure within 2 hours, at a pressure release rate of 0.1 MPa/min, and keep it at normal pressure for 2 hours;
  • Step 5 Fill with nitrogen to 0.2MPa, open the discharge valve, the material is pelletized by the injection lead, cold water tank, and pelletizer.
  • the cold water tank is used to cool the material. It is cooled from soft and tough state to brittle and hard state for easy cutting.
  • the speed of the pelletizer is fast or slow, the size of the resin particles is controlled, and the nylon resin is obtained by vacuum drying to a moisture content of ⁇ 0.5%.
  • Toughness The spline is constantly folded in half.
  • the sixth step adding nylon resin to 1% by mass of antioxidant 1010 and 10% by mass of titanium dioxide, modified by an extruder, dried, and then crushed and sieved to obtain nylon powder;
  • Step 7 Prepare encapsulated buckle embryos from nylon powder, then heat the embryos into the vibrating plate, powder the embryos, and heat the powdered embryos with heating belts and calender them to obtain nylon encapsulated buckles.
  • the acid dyes dye it at 60°C for 30 minutes, then wash it with water.
  • Coating color The color is gorgeous, no white spots, no stains, high gloss, smooth surface; outdoor sunshine for 30 days, no obvious change in color.
  • nylon encapsulated buttons An important indicator of nylon encapsulated buttons is dyeing in acid dyes. After dyeing, the surface color of nylon encapsulated buttons must be uniform without white spots and stains. Therefore, the adjustment of the dyeing process is particularly important.
  • low-concentration acid dye aqueous solutions should be used, the concentration should be controlled between 0.5% and 1.5%, the dyeing temperature should be controlled between 60 and 70°C, and the dyeing time should be controlled between 20 and 30 minutes to ensure coating.
  • the surface of the layer is evenly dyed and the color fastness, and it is easy to control the dyeing depth of the nylon encapsulated button.
  • high-concentration acid dye aqueous solution should be used, the concentration should be controlled between 1.5% and 5%, the dyeing temperature should be controlled between 70 and 90°C, and the dyeing time should be controlled between 20 and 30 minutes to ensure coating.
  • the layer surface is dyed evenly and color fastness.

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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)
  • Life Sciences & Earth Sciences (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Polyamides (AREA)

Abstract

一种尼龙粉末的制备方法及应用，由己二胺、癸二胺、己二酸、癸二酸、十二碳二酸和己内酰胺按不同的质量份数配比混合均匀，添加添加剂进行聚合反应制得尼龙树脂，然后经机械制粉或化学制粉制得尼龙粉末。由本产品制得的尼龙包胶扣具有染色速度可控，颜色艳丽，色牢度高，成本低等优点，可广泛应用于内衣尼龙包胶扣行业。

Description

一种尼龙粉末的制备方法及应用 技术领域
本发明属于尼龙材料技术领域，特别涉及一种尼龙粉末的制备方法及应用。
背景技术
内衣用包胶扣，采用尼龙包胶，具有无毒、防锈、耐盐雾、涂层艳丽，易染色、色牢度高等特点，在内衣包胶扣领域广泛应用。目前主要以国外的尼龙11为主，国内也有尼龙1010和尼龙1012制备的尼龙粉末应用于该领域，但成本偏高，不利于推广。
发明内容
解决的技术问题：本申请主要是提出一种尼龙粉末的制备方法及应用，解决现有技术中存在的成本偏高，不利于推广等技术问题，具有原料易得，成本低，性能优良，便于制备的特点。
技术方案：
一种尼龙粉末的制备方法，包括如下步骤：
第一步：称取己二胺、癸二胺、己二酸、癸二酸、十二碳二酸和己内酰胺原料，所述原料具体称量方式为按质量份数配比称取己二胺∶癸二酸∶己内酰胺＝(29～32)∶(51～58)∶(10～20)或己二胺∶十二碳二酸∶己内酰胺＝(24～30)∶(56～65)∶(5～15)或己二胺∶癸二酸∶己二酸＝(37～38)∶(48～57)∶(6～14)或己二胺∶十二碳二酸∶己二酸＝(34～36)∶(53～63)∶(3～11)或己二胺∶癸二胺∶癸二酸＝(26～33)∶(4～14)∶(60～63)或己二胺∶癸二胺∶十二碳二酸＝(23～30)∶(4～13)∶(64～66)或癸二胺∶癸二酸∶己内酰胺＝(4～14)∶(6～16)∶(70～90)或癸二胺∶十二碳二酸∶己内酰胺＝(2～10)∶(3～11)∶(75～95)；
第二步：在原料中添加原料总质量2.1-7.5％的添加剂，混合均匀得混合料；
第三步：将混合料投入高压反应釜，密封，氮气置换，将釜内空气排出，充氮气至0.05-0.2MPa，升温，当料温升至200℃，压力达到1.2MPa时开始保温保压，时间2小时；
第四步：然后在2小时内将压力均匀泄至常压，并在常压下保温2小时；
第五步：充入氮气至0.2MPa，开启出料阀，物料经注带头、冷水槽、切粒机切粒，经真空干燥，即得尼龙树脂；
第六步：将尼龙树脂通过机械制粉或化学制粉制得尼龙粉末。
作为本发明的一种优选技术方案：所述第二步中添加剂为抗氧剂、光亮剂、表面处理剂和分子量调节剂。
作为本发明的一种优选技术方案：所述抗氧剂为复配抗氧剂，按质量份数配比为亚磷酸∶抗氧剂1098∶抗氧剂168＝(1～5)∶(5～10)∶(5～10)，其加入量为混合料总质量的1～3％。
作为本发明的一种优选技术方案：所述光亮剂为复配光亮剂，按质量份数配比为聚醚改性水溶性硅油∶安息香∶硬脂酸钙＝(0.1～0.5)∶(1～5)∶(1～5)，其加入量为混合料总质量的0.5～2％。
作为本发明的一种优选技术方案：所述表面处理剂，为阴离子型表面活性剂的一种或几种复配物，所述阴离子型表面活性剂如十二烷基苯磺酸钠，其加入量为混合料总质量的0.5～2％。
作为本发明的一种优选技术方案：所述分子量调节剂为己二酸，加入量为混合料总质量的0.1～0.5％。
作为本发明的一种优选技术方案：所述第二步中混合速度为1000-2000r/min，混合时间为2-5min，第四步中泄压速度为0.02-0.12MPa/min，第五步中真空干燥至含水率＜0.5％。
作为本发明的一种优选技术方案：所述第六步中机械制粉步骤为将尼龙树脂加入1％质量比的抗氧剂1010和10％质量比的钛白粉，经挤出机改性，烘干后经过深冷粉碎，筛粉，制得尼龙粉末。
作为本发明的一种优选技术方案：所述第六步中化学制粉步骤为将尼龙树脂投入高压反应釜，加入1％质量比的抗氧剂1010和10％质量比的钛白粉，加入96％的乙醇，所述乙醇重量为尼龙树脂重量的3-4倍，经170-180℃高温溶解，降温析出，离心分离，烘干，筛粉，制得尼龙粉末。
另外，本发明还提供了所述尼龙粉末的制备方法制备得到的尼龙粉末在制备尼龙包胶扣上的应用。
有益效果：本申请所述尼龙粉末的制备方法及应用采用以上技术方案与现有技术相比，具有以下技术效果：
1、合成尼龙树脂原料的全部国产化，不仅尼龙树脂的性能比原来得到提升，也降低了生 产成本，确保了原料的供应充足。
2、具有原料易得，成本低，性能优良，便于制备的特点。
3、产品熔点172～190℃，熔融指数(230℃，2.16kg)：40-56克/10分钟，硬度(邵氏硬度)：68-70，韧性：样条对折不断。
4、涂层颜色：颜色艳丽，无白点、无色斑，涂层光泽度高，表面滑爽。
5、包胶扣户外日照30天，色泽无明显改变。
6、拉伸强度55-75MPa，弯曲强度75-95MPa，缺口冲击强度45-55J/m，耐磨性和耐酸碱腐蚀性能好，耐磨性摩擦系数低于0.2，PV值高，泰伯磨耗1-3mg/1000次，通过DIN53754测得磨耗量1-3mg，自润滑性好和耐盐雾，耐油，耐-60℃低温。
具体实施方式
下面结合实施例对本发明做进一步说明。
实施例1
一种尼龙粉末的制备方法，包括如下步骤：
第一步：按质量份数配比称取己二胺87公斤，癸二酸153公斤，己内酰胺60公斤，抗氧剂4.5公斤，光亮剂1.5公斤，十二烷基苯磺酸钠1公斤，己二酸600克，所述抗氧剂由亚磷酸500克、抗氧剂1098为2公斤和抗氧剂168为2公斤复配而成，所述光亮剂由硬脂酸钙500克、聚醚改性水溶性硅油500克和安息香500克复配而成；
第二步：混合均匀得混合料，混合速度为1000-2000r/min，混合时间为2-5min；
第三步：将混合料投入高压反应釜，密封，氮气置换，将釜内空气排出，充氮气至0.2MPa，升温，当料温升至200℃，压力达到1.2MPa时开始保温保压，时间2小时；
第四步：然后在2小时内将压力均匀泄至常压，泄压速度为0.1MPa/min，并在常压下保温2小时；
第五步：充入氮气至0.2MPa，开启出料阀，物料经注带头、冷水槽、切粒机切粒，经真空干燥至含水率＜0.5％，即得尼龙树脂。
尼龙树脂产品指标如下：
熔点：175～185℃
熔融指数(230℃，2.16kg)：50克/10分钟
硬度(邵氏硬度)：70
韧性：样条对折不断。
第六步：将尼龙树脂加入1％质量比的抗氧剂1010和10％质量比的钛白粉，经挤出机改性，烘干后经过深冷粉碎，筛粉，制得尼龙粉末；
第七步：将尼龙粉末制备尼龙包胶扣，首先制备包胶扣胚胎，然后将胚胎加热后进入振动盘，将胚胎上粉，上粉后的胚胎经加热带加热，压光，得到尼龙包胶扣，在浓度为1％的酸性染料中，于80℃染色20分钟，然后经水洗即得。
检测结果如下：
涂层颜色：颜色艳丽，无白点、无色斑，涂层光泽度高，表面滑爽；包胶扣户外日照30天，色泽无明显改变。
实施例2
一种尼龙粉末的制备方法，包括如下步骤：
第一步：按质量份数配比称取己二胺90公斤，十二碳二酸180公斤，己内酰胺30公斤，抗氧剂3.5公斤，光亮剂2公斤，十二烷基苯磺酸钠0.5公斤，己二酸800克，所述抗氧剂由亚磷酸500克、抗氧剂1098 2公斤和抗氧剂168 1公斤复配而成，所述光亮剂由硬脂酸钙500克、聚醚改性水溶性硅油1000克和安息香500克复配而成；
第二步：混合均匀得混合料，混合速度为1000-2000r/min，混合时间为2-5min；
第三步：将混合料投入高压反应釜，密封，氮气置换，将釜内空气排出，充氮气至0.2MPa，升温，当料温升至200℃，压力达到1.2MPa时开始保温保压，时间2小时；
第四步：然后在2小时内将压力均匀泄至常压，泄压速度为0.1MPa/min，并在常压下保温2小时；
第五步：充入氮气至0.2MPa，开启出料阀，物料经注带头、冷水槽、切粒机切粒，经真空干燥至含水率＜0.5％，即得尼龙树脂。
尼龙树脂产品指标如下：
熔点：1780～190℃
熔融指数(230℃，2.16kg)：40克/10分钟
硬度(邵氏硬度)：68
韧性：样条对折不断。
第六步：将尼龙树脂投入高压反应釜，加入1％质量比的抗氧剂1010和10％质量比的，放入96％的乙醇，所述乙醇重量为尼龙树脂重量的3-4倍，经170-180℃高温溶解，降温析出，离 心分离，烘干，筛粉，制得尼龙粉末；
第七步：将尼龙粉末制备尼龙包胶扣，首先制备包胶扣胚胎，然后将胚胎加热后进入振动盘，将胚胎上粉，上粉后的胚胎经加热带加热，压光，得到尼龙包胶扣，在浓度为2％的酸性染料中，于70℃染色20分钟，然后经水洗即得。
检测结果如下：
涂层颜色：颜色艳丽，无白点、无色斑，涂层光泽度高，表面滑爽；包胶扣户外日照30天，色泽无明显改变。
实施例3
一种尼龙粉末的制备方法，包括如下步骤：
第一步：按质量份数配比称取己二胺114公斤，癸二酸144公斤，己二酸42公斤，抗氧剂3公斤，光亮剂1.5公斤，十二烷基苯磺酸钠1.5公斤，己二酸500克，所述抗氧剂由亚磷酸500克、抗氧剂1098 2公斤和抗氧剂168 0.5公斤复配而成，所述光亮剂由硬脂酸钙500克、聚醚改性水溶性硅油500克和安息香500克复配而成；
第二步：混合均匀得混合料，混合速度为1000-2000r/min，混合时间为2-5min；
第三步：将混合料投入高压反应釜，密封，氮气置换，将釜内空气排出，充氮气至0.2MPa，升温，当料温升至200℃，压力达到1.2MPa时开始保温保压，时间2小时；
第四步：然后在2小时内将压力均匀泄至常压，泄压速度为0.1MPa/min，并在常压下保温2小时；
第五步：充入氮气至0.2MPa，开启出料阀，物料经注带头、冷水槽、切粒机切粒，冷水槽用于冷却物料，由软韧状态冷却为脆硬状态，便于切料，切粒机转速快慢，控制树脂颗粒大小，经真空干燥至含水率＜0.5％，即得尼龙树脂。
尼龙树脂产品指标如下：
熔点：172～182℃
熔融指数(230℃，2.16kg)：56克/10分钟
硬度(邵氏硬度)：70
韧性：样条对折不断。
第六步：将尼龙树脂加入1％质量比的抗氧剂1010和10％质量比的钛白粉，经挤出机改性，烘干后经过深冷粉碎，筛粉，制得尼龙粉末；
第七步：将尼龙粉末制备包胶扣胚胎，然后将胚胎加热后进入振动盘，将胚胎上粉，上 粉后的胚胎经加热带加热，压光，得到尼龙包胶扣，在浓5％的酸性染料中，于60℃染色30分钟，然后经水洗即得。
检测结果如下：
涂层颜色：颜色艳丽，无白点、无色斑，涂层光泽度高，表面滑爽；包胶扣户外日照30天，色泽无明显改变。
尼龙包胶扣的重要指标是在酸性染料中的染色，染色后尼龙包胶扣表面颜色要均匀，不能有白点和色斑，因此，染色工艺的调整尤为重要。
对于染色速度快的树脂，要采用低浓度的酸性染料水溶液，浓度控制在0.5％～1.5％之间，染色温度控制在60～70℃之间，染色时间控制在20～30分钟，才能确保涂层表面染色均匀和色牢度，而且也容易控制尼龙包胶扣的染色深浅程度。
对于染色速度慢的树脂，要采用高浓度的酸性染料水溶液，浓度控制在1.5％～5％之间，染色温度控制在70～90℃之间，染色时间控制在20～30分钟，才能确保涂层表面染色均匀和色牢度。
上述实施例只是列举了本专利中的部分原料配比，在此不再一一列举。在不背离本申请精神和实质的情况下，对本申请方法、步骤或条件所作的修改和替换，均属于本申请的范围。

Claims (10)

  1. 一种尼龙粉末的制备方法，其特征在于包括如下步骤：
    第一步：称取己二胺、癸二胺、己二酸、癸二酸、十二碳二酸和己内酰胺原料，所述原料具体称量方式为按质量份数配比称取己二胺∶癸二酸∶己内酰胺＝(29～32)∶(51～58)∶(10～20)或己二胺∶十二碳二酸∶己内酰胺＝(24～30)∶(56～65)∶(5～15)或己二胺∶癸二酸∶己二酸＝(37～38)∶(48～57)∶(6～14)或己二胺∶十二碳二酸∶己二酸＝(34～36)∶(53～63)∶(3～11)或己二胺∶癸二胺∶癸二酸＝(26～33)∶(4～14)∶(60～63)或己二胺∶癸二胺∶十二碳二酸＝(23～30)∶(4～13)∶(64～66)或癸二胺∶癸二酸∶己内酰胺＝(4～14)∶(6～16)∶(70～90)或癸二胺∶十二碳二酸∶己内酰胺＝(2～10)∶(3～11)∶(75～95)；
    第二步：在原料中添加原料总质量2.1-7.5％的添加剂，混合均匀得混合料；
    第三步：将混合料投入高压反应釜，密封，氮气置换，将釜内空气排出，充氮气至0.05-0.2MPa，升温，当料温升至200℃，压力达到1.2MPa时开始保温保压，时间2小时；
    第四步：然后在2小时内将压力均匀泄至常压，并在常压下保温2小时；
    第五步：充入氮气至0.2MPa，开启出料阀，物料经注带头、冷水槽、切粒机切粒，经真空干燥，即得尼龙树脂；
    第六步：将尼龙树脂通过机械制粉或化学制粉制得尼龙粉末。
  2. 根据权利要求1所述尼龙粉末的制备方法，其特征在于：所述第二步中添加剂为抗氧剂、光亮剂、表面处理剂和分子量调节剂。
  3. 根据权利要求2所述尼龙粉末的制备方法，其特征在于：所述抗氧剂为复配抗氧剂，按质量份数配比为亚磷酸∶抗氧剂1098∶抗氧剂168＝(1～5)∶(5～10)∶(5～10)，其加入量为混合料总质量的1～3％。
  4. 根据权利要求2所述尼龙粉末的制备方法，其特征在于：所述光亮剂为复配光亮剂，按质量份数配比为聚醚改性水溶性硅油∶安息香∶硬脂酸钙＝(0.1～0.5)∶(1～5)∶(1～5)，其加入量为混合料总质量的0.5～2％。
  5. 根据权利要求2所述尼龙粉末的制备方法，其特征在于：所述表面处理剂，为阴离子型表面活性剂的一种或几种复配物，所述阴离子型表面活性剂如十二烷基苯磺酸钠，其加入量为混合料总质量的0.5～2％。
  6. 根据权利要求2所述尼龙粉末的制备方法，其特征在于：所述分子量调节剂为己二酸，加 入量为混合料总质量的0.1～0.5％。
  7. 根据权利要求1述尼龙粉末的制备方法，其特征在于：所述第二步中混合速度为1000-2000r/min，混合时间为2-5min，第四步中泄压速度为0.02-0.12MPa/min，第五步中真空干燥至含水率＜0.5％。
  8. 根据权利要求1所述尼龙粉末的制备方法，其特征在于：所述第六步中机械制粉步骤为将尼龙树脂加入1％质量比的抗氧剂1010和10％质量比的钛白粉，经挤出机改性，烘干后经过深冷粉碎，筛粉，制得尼龙粉末。
  9. 根据权利要求1所述尼龙粉末的制备方法，其特征在于：所述第六步中化学制粉步骤为将尼龙树脂投入高压反应釜，加入1％质量比的抗氧剂1010和10％质量比的钛白粉，加入96％的乙醇，所述乙醇重量为尼龙树脂重量的3-4倍，经170-180℃高温溶解，降温析出，离心分离，烘干，筛粉，制得尼龙粉末。
  10. 一种权利要求1所述尼龙粉末的制备方法制备得到的尼龙粉末在制备尼龙包胶扣上的应用。
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