WO2017214746A1 - 超轻型聚氨酯树脂的配方及制备工艺 - Google Patents

超轻型聚氨酯树脂的配方及制备工艺 Download PDF

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WO2017214746A1
WO2017214746A1 PCT/CN2016/000330 CN2016000330W WO2017214746A1 WO 2017214746 A1 WO2017214746 A1 WO 2017214746A1 CN 2016000330 W CN2016000330 W CN 2016000330W WO 2017214746 A1 WO2017214746 A1 WO 2017214746A1
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parts
temperature
polyurethane resin
powder
ultra
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PCT/CN2016/000330
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French (fr)
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杨磊
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杨磊
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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
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • 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
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step

Definitions

  • the invention relates to the technical field of polyurethane resin production, in particular to a formula and a preparation process of an ultra-light polyurethane resin.
  • Polyurethane material is the abbreviation of polyurethane, the English name is polyurethane, which is a polymer material.
  • Polyurethane is an emerging organic polymer material, which is known as the “fifth largest plastic” and is widely used in many fields of the national economy due to its excellent performance.
  • the application fields of the products include light industry, chemical industry, electronics, textile, medical, construction, building materials, automobile, national defense, aerospace, aviation, etc.
  • Polyurethane slurry is used as a coating to prepare polyurethane synthetic leather and artificial leather.
  • Polyurethane synthetic leather has soft and natural luster, soft handfeel and strong leathery appearance.
  • the present invention provides an ultra-light polyurethane resin formulation and preparation process, which has a lower density, can float well on water, and is used for the production of gloves, so that the glove has better friction performance. It is worth promoting.
  • a formulation of an ultra-light polyurethane resin is composed of the following raw materials in parts by weight:
  • top polymer 40-50 parts of toluene diisocyanate, 30-40 parts of polymethylene polyphenyl polyisocyanate, 10-20 parts of reactive emulsifier, 10-14 parts of dianhydride, diamine 10 -14 parts, 8-10 parts of phosphoric acid, 4-6 parts of talc.
  • the following raw materials are composed by weight:
  • top polymer 80 parts of top polymer, 40 parts of toluene diisocyanate, 30 parts of polymethylene polyphenyl polyisocyanate, 10 parts of reactive emulsifier, 10 parts of dianhydride, 10 parts of diamine, 8 parts of phosphoric acid, 4 parts of talc .
  • the following raw materials are composed by weight:
  • top polymer 85 parts of top polymer, 45 parts of toluene diisocyanate, 35 parts of polymethylene polyphenyl polyisocyanate, 15 parts of reactive emulsifier, 12 parts of dianhydride, 12 parts of diamine, 9 parts of phosphoric acid, 5 parts of talc .
  • the following raw materials are composed by weight:
  • top polymer 50 parts of toluene diisocyanate, 40 parts of polymethylene polyphenyl polyisocyanate, 20 parts of reactive emulsifier, 14 parts of dianhydride, 14 parts of diamine, 10 parts of phosphoric acid, 6 parts of talc .
  • the prepolymerization method of the top polymer after the top polymer is taken out, mixed with the dibasic anhydride and the diamine, ground into a powder, mixed and stirred, and heated while stirring. After the heating and dehydration reaction, the foaming is carried out, and the material after foaming is cooled and dried for 30 min to 45 min, and the heating process ensures that the temperature is 480 ° C - 630 ° C.
  • the invention also designs a preparation process of an ultra-light polyurethane resin, comprising the following steps:
  • the raw materials are mixed according to the formula, ground into a powder by grinding into a grinder, and the powder is uniformly mixed and stirred in a mixer.
  • the stirring is continued, the temperature is continued until the temperature reaches 98 ° C, the heating is stopped, and the powder is poured out.
  • stirred raw material is added into the heat preservation tank, kept at a temperature of 115 ° C for 40 min to 50 min, and stirred and dehydrated at a vacuum of 680 mmHg-710 mmHg for 1.5 h.
  • the finished product is ground into a powder, and the density of the finished product is measured by adding an electron densitometer.
  • the speed of the mixer in the step (1) is 45r/min, the mixing direction of the mixer is changed every 3 minutes.
  • the invention adopts the heating dehydration reaction to pretreat the top polymer, improves the polymer density inside the top polymer, can be well applied to the manufacture of the glove, and the manufactured glove has better friction performance and the density is smaller. It floats well on the water and is worth promoting.
  • An ultra-light polyurethane resin formulation consisting of the following materials in parts by weight:
  • top polymer 80 parts of top polymer, 40 parts of toluene diisocyanate, 30 parts of polymethylene polyphenyl polyisocyanate, 10 parts of reactive emulsifier, 10 parts of dianhydride, 10 parts of diamine, 8 parts of phosphoric acid, 4 parts of talc .
  • the pretreatment method of the top polymer after taking out the top polymer, mixing with the dibasic anhydride and the diamine, grinding into a powder, mixing and stirring, heating while stirring, foaming after heating and dehydrating, after foaming
  • the material is cooled and dried for 30min-45min, and the heating process ensures the temperature is 480°C-630°C;
  • the preparation process comprises the following steps:
  • the raw materials are mixed according to the formula, ground into a powder by grinding into a grinder, and the powder is uniformly mixed and stirred in a mixer.
  • the stirring is continued, the temperature is continued until the temperature reaches 98 ° C, the heating is stopped, and the powder is poured out.
  • stirred raw material is added into the heat preservation tank, kept at a temperature of 115 ° C for 40 min to 50 min, and stirred and dehydrated at a vacuum of 680 mmHg-710 mmHg for 1.5 h.
  • the finished product is ground into a powder, and the density of the finished product is measured by adding an electron densitometer.
  • An ultra-light polyurethane resin formulation consisting of the following materials in parts by weight:
  • top polymer 85 parts of top polymer, 45 parts of toluene diisocyanate, 35 parts of polymethylene polyphenyl polyisocyanate, 15 parts of reactive emulsifier, 12 parts of dianhydride, 12 parts of diamine, 9 parts of phosphoric acid, 5 parts of talc .
  • the pretreatment method of the top polymer after taking out the top polymer, mixing with the dibasic anhydride and the diamine, grinding into a powder, mixing and stirring, heating while stirring, foaming after heating and dehydrating, after foaming
  • the material is cooled and dried for 30min-45min, and the heating process ensures the temperature is 480°C-630°C;
  • the preparation process comprises the following steps:
  • the raw materials are mixed according to the formula, ground into a powder by grinding into a grinder, and the powder is uniformly mixed and stirred in a mixer.
  • the stirring is continued, the temperature is continued until the temperature reaches 98 ° C, the heating is stopped, and the powder is poured out.
  • stirred raw material is added into the heat preservation tank, kept at a temperature of 115 ° C for 40 min to 50 min, and stirred and dehydrated at a vacuum of 680 mmHg-710 mmHg for 1.5 h.
  • the finished product is ground into a powder, and the density of the finished product is measured by adding an electron densitometer.
  • An ultra-light polyurethane resin formulation consisting of the following materials in parts by weight:
  • top polymer 50 parts of toluene diisocyanate, 40 parts of polymethylene polyphenyl polyisocyanate, 20 parts of reactive emulsifier, 14 parts of dianhydride, 14 parts of diamine, 10 parts of phosphoric acid, 6 parts of talc .
  • the pretreatment method of the top polymer after taking out the top polymer, mixing with the dibasic anhydride and the diamine, grinding into a powder, mixing and stirring, heating while stirring, foaming after heating and dehydrating reaction, The material after foaming is cooled and dried for 30min-45min, and the heating process ensures the temperature is 480°C-630°C;
  • the preparation process comprises the following steps:
  • the raw materials are mixed according to the formula, ground into a powder by grinding into a grinder, and the powder is uniformly mixed and stirred in a mixer.
  • the stirring is continued, the temperature is continued until the temperature reaches 98 ° C, the heating is stopped, and the powder is poured out.
  • stirred raw material is added into the heat preservation tank, kept at a temperature of 115 ° C for 40 min to 50 min, and stirred and dehydrated at a vacuum of 680 mmHg-710 mmHg for 1.5 h.
  • the finished product is ground into a powder, and the density of the finished product is measured by adding an electron densitometer.
  • the invention has the advantages that the pretreatment of the top polymer by the heating dehydration reaction improves the polymer density inside the top polymer, and can be well applied to the manufacture of gloves, and the gloves are more manufactured. Good friction performance, smaller density can float well on the water, it is worth promoting.

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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)
  • Polyurethanes Or Polyureas (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

一种超轻型聚氨酯树脂的配方，按照重量份数由如下原料组成：顶聚体80-90份，甲苯二异氰酸酯40-50份，多亚甲基多苯基多异氰酸酯30-40份，活性乳化剂10-20份，二元酐10-14份，二元胺10-14份，磷酸8-10份，滑石粉4-6份，其制备工艺为：按配方将原料混合，加入研磨机内研磨成粉末，将粉末混合均匀加入搅拌机内搅拌，搅拌的时候持续加温，直到温度达到98℃，将粉末倒出，加入保温罐内，保持115℃的温度保温40min-50min，在680mmHg-710mmHg真空度下进行搅拌脱水1.5h，在氮气的保护下，再次进行搅拌，降低温度至40℃，加入催化剂重新加热，保持加热温度为90℃，降温至50℃，加入稀释剂之后乳化45min，采用减压蒸馏法脱除稀释剂，导入模具中成型，之后进行干燥处理，具有很小的密度，值得推广。

Description

[根据细则37.2由ISA制定的发明名称]　超轻型聚氨脂树脂的配方及制备工艺 技术领域
本发明涉及聚氨脂树脂生产技术领域，具体涉及一种超轻型聚氨脂树脂的配方及制备工艺。
背景技术
聚氨酯材料是聚氨基甲酸酯的简称，英文名称是polyurethane，它是一种高分子材料。聚氨酯是一种新兴的有机高分子材料，被誉为“第五大塑料”，因其卓越的性能而被广泛应用于国民经济众多领域。产品应用领域涉及轻工、化工、电子、纺织、医疗、建筑、建材、汽车、国防、航天、航空等，聚氨酯浆料用作涂层制备聚氨酯合成革、人造革。聚氨酯合成革具有光泽柔和、自然，手感柔软，真皮感强的外观，具有与基材粘接性能优异、抗磨损、耐挠曲、抗老化、抗霉菌性好等优异的机械性能，同时还具备耐寒性好、透气、可洗涤、加工方便、价格优廉等优点，是天然皮革的最为理想的替代品，广泛应用于服装、制鞋、箱包、家具、体育等行业。随着社会的发展，现在很多的手套采用了聚氨脂材料制成。随着社会的发展，越来越多的手套采用了聚氨脂来制造，但是现有的很多的聚氨脂树脂材料，密度都过高，在水中的时候会沉下去，因此设计了一种超轻型聚氨脂树脂。
发明内容
针对以上问题，本发明提供了一种超轻型聚氨脂树脂的配方及制备工艺，具有更低的密度，能很好的漂浮在水上，用于手套的生产，使得手套具有更好的摩擦性能，值得推广。
为了实现上述目的，本发明采用的技术方案如下：一种超轻型聚氨脂树脂的配方，按照重量份数由如下原料组成：
顶聚体80-90份，甲苯二异氰酸酯40-50份，多亚甲基多苯基多异氰酸酯30-40份，活性乳化剂10-20份，二元酐10-14份，二元胺10-14份，磷酸8-10份，滑石粉4-6份。
作为本发明一种优选的技术方案，按照重量份数由如下原料组成：
顶聚体80份，甲苯二异氰酸酯40份，多亚甲基多苯基多异氰酸酯30份，活性乳化剂10份，二元酐10份，二元胺10份，磷酸8份，滑石粉4份。
作为本发明一种优选的技术方案，按照重量份数由如下原料组成：
顶聚体85份，甲苯二异氰酸酯45份，多亚甲基多苯基多异氰酸酯35份，活性乳化剂15份，二元酐12份，二元胺12份，磷酸9份，滑石粉5份。
作为本发明一种优选的技术方案，按照重量份数由如下原料组成：
顶聚体90份，甲苯二异氰酸酯50份，多亚甲基多苯基多异氰酸酯40份，活性乳化剂20份，二元酐14份，二元胺14份，磷酸10份，滑石粉6份。
作为本发明一种优选的技术方案，所述顶聚体的预处理方法：将顶聚体取出之后，与二元酐和二元胺混合，研磨成粉末后混合搅拌，边搅拌边加热，经过加热脱水反应之后发泡，发泡之后的材料进行冷却晾干30min-45min，加热过程保证温度为480℃-630℃。
另外本发明还设计了一种超轻型聚氨脂树脂的制备工艺，包括如下步骤：
(1)按配方将原料混合，加入研磨机内研磨成粉末，将粉末混合均匀加入搅拌机内搅拌，搅拌的时候持续加温，直到温度达到98℃，停止加热，将粉末倒出。
(2)将搅拌好的原料加入保温罐内，保持115℃的温度保温40min-50min，在680mmHg-710mmHg真空度下进行搅拌脱水1.5h。
(3)脱水之后在氮气的保护下，再次进行搅拌，降低温度至40℃，加入催化剂重新加热，保持加热温度为90℃。
(4)降温至50℃，加入稀释剂之后乳化45min，采用减压蒸馏法脱除稀释剂，导入模具中成型，之后进行干燥处理。
(5)将成品研磨成粉末，加入电子密度计中测量成品密度。
作为本发明一种优选的技术方案，所述步骤(1)中搅拌机转速为 45r/min，搅拌机搅拌方向每3min变换一次。
本发明的有益效果：
本发明采用加热脱水反应对顶聚体进行预处理，提高了顶聚体内部的聚合物密度，能很好的应用于手套的制造，制造出的手套具有更好的摩擦性能，密度更小可以很好的漂浮在水面上，值得推广。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
实施例1：
一种超轻型聚氨脂树脂的配方，按照重量份数由如下原料组成：
顶聚体80份，甲苯二异氰酸酯40份，多亚甲基多苯基多异氰酸酯30份，活性乳化剂10份，二元酐10份，二元胺10份，磷酸8份，滑石粉4份。
所述顶聚体的预处理方法：将顶聚体取出之后，与二元酐和二元胺混合，研磨成粉末后混合搅拌，边搅拌边加热，经过加热脱水反应之后发泡，发泡之后的材料进行冷却晾干30min-45min，加热过程保证温度为480℃-630℃；
其制备工艺包括如下步骤：
(1)按配方将原料混合，加入研磨机内研磨成粉末，将粉末混合均匀加入搅拌机内搅拌，搅拌的时候持续加温，直到温度达到98℃，停止加热，将粉末倒出。
(2)将搅拌好的原料加入保温罐内，保持115℃的温度保温40min-50min，在680mmHg-710mmHg真空度下进行搅拌脱水1.5h。
(3)脱水之后在氮气的保护下，再次进行搅拌，降低温度至40℃，加入催化剂重新加热，保持加热温度为90℃。
(4)降温至50℃，加入稀释剂之后乳化45min，采用减压蒸馏法脱除稀释剂，导入模具中成型，之后进行干燥处理。
(5)将成品研磨成粉末，加入电子密度计中测量成品密度。
实施例2：
一种超轻型聚氨脂树脂的配方，按照重量份数由如下原料组成：
顶聚体85份，甲苯二异氰酸酯45份，多亚甲基多苯基多异氰酸酯35份，活性乳化剂15份，二元酐12份，二元胺12份，磷酸9份，滑石粉5份。
所述顶聚体的预处理方法：将顶聚体取出之后，与二元酐和二元胺混合，研磨成粉末后混合搅拌，边搅拌边加热，经过加热脱水反应之后发泡，发泡之后的材料进行冷却晾干30min-45min，加热过程保证温度为480℃-630℃；
其制备工艺包括如下步骤：
(1)按配方将原料混合，加入研磨机内研磨成粉末，将粉末混合均匀加入搅拌机内搅拌，搅拌的时候持续加温，直到温度达到98℃，停止加热，将粉末倒出。
(2)将搅拌好的原料加入保温罐内，保持115℃的温度保温40min-50min，在680mmHg-710mmHg真空度下进行搅拌脱水1.5h。
(3)脱水之后在氮气的保护下，再次进行搅拌，降低温度至40℃，加入催化剂重新加热，保持加热温度为90℃。
(4)降温至50℃，加入稀释剂之后乳化45min，采用减压蒸馏法脱除稀释剂，导入模具中成型，之后进行干燥处理。
(5)将成品研磨成粉末，加入电子密度计中测量成品密度。
实施例3：
一种超轻型聚氨脂树脂的配方，按照重量份数由如下原料组成：
顶聚体90份，甲苯二异氰酸酯50份，多亚甲基多苯基多异氰酸酯40份，活性乳化剂20份，二元酐14份，二元胺14份，磷酸10份，滑石粉6份。
所述顶聚体的预处理方法：将顶聚体取出之后，与二元酐和二元胺混合，研磨成粉末后混合搅拌，边搅拌边加热，经过加热脱水反应之后发泡， 发泡之后的材料进行冷却晾干30min-45min，加热过程保证温度为480℃-630℃；
其制备工艺包括如下步骤：
(1)按配方将原料混合，加入研磨机内研磨成粉末，将粉末混合均匀加入搅拌机内搅拌，搅拌的时候持续加温，直到温度达到98℃，停止加热，将粉末倒出。
(2)将搅拌好的原料加入保温罐内，保持115℃的温度保温40min-50min，在680mmHg-710mmHg真空度下进行搅拌脱水1.5h。
(3)脱水之后在氮气的保护下，再次进行搅拌，降低温度至40℃，加入催化剂重新加热，保持加热温度为90℃。
(4)降温至50℃，加入稀释剂之后乳化45min，采用减压蒸馏法脱除稀释剂，导入模具中成型，之后进行干燥处理。
(5)将成品研磨成粉末，加入电子密度计中测量成品密度。
样品号 标准品 实施例1 实施例2 实施例3
密度g/cm3 1.04 0.78 0.75 0.70
由上表可知，实施例1至实施例3所得成品的密度都优于标准品，性能优于标准品。
基于上述，本发明的优点在于，本发明采用加热脱水反应对顶聚体进行预处理，提高了顶聚体内部的聚合物密度，能很好的应用于手套的制造，制造出的手套具有更好的摩擦性能，密度更小可以很好的漂浮在水面上，值得推广。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (7)

  1. 一种超轻型聚氨脂树脂的配方，其特征在于，按照重量份数由如下原料组成：
    顶聚体80-90份，甲苯二异氰酸酯40-50份，多亚甲基多苯基多异氰酸酯30-40份，活性乳化剂10-20份，二元酐10-14份，二元胺10-14份，磷酸8-10份，滑石粉4-6份。
  2. 根据权利要求1所述的一种超轻型聚氨脂树脂的配方，其特征在于，按照重量份数由如下原料组成：
    顶聚体80份，甲苯二异氰酸酯40份，多亚甲基多苯基多异氰酸酯30份，活性乳化剂10份，二元酐10份，二元胺10份，磷酸8份，滑石粉4份。
  3. 根据权利要求1所述的一种超轻型聚氨脂树脂的配方，其特征在于，按照重量份数由如下原料组成：
    顶聚体85份，甲苯二异氰酸酯45份，多亚甲基多苯基多异氰酸酯35份，活性乳化剂15份，二元酐12份，二元胺12份，磷酸9份，滑石粉5份。
  4. 根据权利要求1所述的一种超轻型聚氨脂树脂的配方，其特征在于，按照重量份数由如下原料组成：
    顶聚体90份，甲苯二异氰酸酯50份，多亚甲基多苯基多异氰酸酯40份，活性乳化剂20份，二元酐14份，二元胺14份，磷酸10份，滑石粉6份。
  5. 根据权利要求1所述的一种超轻型聚氨脂树脂的配方，其特征在于，所述顶聚体的预处理方法：将顶聚体取出之后，与二元酐和二元胺混合，研磨成粉末后混合搅拌，边搅拌边加热，经过加热脱水反应之后发泡，发泡之后的材料进行冷却晾干30min-45min，加热过程保证温度为480℃-630℃。
  6. 一种超轻型聚氨脂树脂的制备工艺，其特征在于，包括如下步骤：
    (1)按配方将原料混合，加入研磨机内研磨成粉末，将粉末混合均匀加入搅拌机内搅拌，搅拌的时候持续加温，直到温度达到98℃，停止加热， 将粉末倒出。
    (2)将搅拌好的原料加入保温罐内，保持115℃的温度保温40min-50min，在680mmHg-710mmHg真空度下进行搅拌脱水1.5h。
    (3)脱水之后在氮气的保护下，再次进行搅拌，降低温度至40℃，加入催化剂重新加热，保持加热温度为90℃。
    (4)降温至50℃，加入稀释剂之后乳化45min，采用减压蒸馏法脱除稀释剂，导入模具中成型，之后进行干燥处理。
    (5)将成品研磨成粉末，加入电子密度计中测量成品密度。
  7. 根据权利要求1所述的一种超轻型聚氨脂树脂的制备工艺，其特征在于，所述步骤(1)中搅拌机转速为45r/min，搅拌机搅拌方向每3min变换一次。
PCT/CN2016/000330 2016-06-13 2016-06-22 超轻型聚氨酯树脂的配方及制备工艺 WO2017214746A1 (zh)

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