WO2022001557A1 - 一种高弹性尼龙及其制备方法 - Google Patents

一种高弹性尼龙及其制备方法 Download PDF

Info

Publication number
WO2022001557A1
WO2022001557A1 PCT/CN2021/097722 CN2021097722W WO2022001557A1 WO 2022001557 A1 WO2022001557 A1 WO 2022001557A1 CN 2021097722 W CN2021097722 W CN 2021097722W WO 2022001557 A1 WO2022001557 A1 WO 2022001557A1
Authority
WO
WIPO (PCT)
Prior art keywords
nylon
polyborosiloxane
mixed material
heating
high elastic
Prior art date
Application number
PCT/CN2021/097722
Other languages
English (en)
French (fr)
Inventor
李峰
于钟梅
于海洋
王兆军
Original Assignee
西安匹克玄铠新材料有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 西安匹克玄铠新材料有限公司 filed Critical 西安匹克玄铠新材料有限公司
Priority to JP2022581719A priority Critical patent/JP7422252B2/ja
Publication of WO2022001557A1 publication Critical patent/WO2022001557A1/zh

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
    • C08J9/141Hydrocarbons
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/24Crosslinking, e.g. vulcanising, of macromolecules
    • C08J3/243Two or more independent types of crosslinking for one or more polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/24Crosslinking, e.g. vulcanising, of macromolecules
    • C08J3/246Intercrosslinking of at least two polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0014Use of organic additives
    • C08J9/0023Use of organic additives containing oxygen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0061Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00Foams characterized by the expanding agent
    • C08J2203/14Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/14Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms

Definitions

  • the invention relates to the technical field of nylon elastomer modification methods, in particular to a high-elasticity nylon and a preparation method thereof.
  • Nylon elastomer is a block polyamide elastomer product, which is an engineering polymer.
  • the product has a wide range of hardness and good resilience, and its remarkable processing properties make this product an ideal material for producing parts.
  • Nylon elastomer also has good chemical resistance, heat resistance and weather resistance, and has been widely used in sports equipment, impact-resistant parts, watch casings and other fields.
  • the compression set ratio of the conventional nylon elastic body is poor, and it is difficult to restore the original state after being compressed and deformed.
  • the embodiment of the present invention provides a high-elasticity nylon and a preparation method thereof.
  • the specific technical solutions are as follows:
  • an embodiment of the present invention provides a method for preparing high-elasticity nylon, comprising:
  • nylon, polyborosiloxane, and polyethylene glycol and dry the polyborosiloxane; wherein, the mass ratio of the nylon to the polyborosiloxane is 10-100:1; The mass of ethylene glycol is 10% of the mass of the polyborosiloxane;
  • the nylon, the polyborosiloxane, and the polyethylene glycol are placed in a predetermined device for heating and mixing to obtain a first mixed material; wherein the heating temperature is 150-180° C., and the heating time is 3-5 minutes;
  • the quality of the cyclopentane is the quality of the first mixed material 5-10% of the temperature, the mixing temperature is 150-180°C, and the mixing time is 7-10min;
  • the particulate matter is foamed to obtain high elastic nylon; wherein the foaming temperature is 160-180° C., the foaming time is 5-7min, and the foaming pressure is 140-160kg/cm 2 .
  • the thickness of the sheet is 10 mm.
  • the predetermined device is an extruder.
  • the extruder is a twin-screw extruder or a single-screw extruder.
  • the embodiment of the present invention provides a high-elasticity nylon, which is prepared by the above-mentioned preparation method of the high-elasticity nylon.
  • An embodiment of the present invention provides a method for preparing high-elasticity nylon, including: obtaining nylon, polyborosiloxane, polyethylene glycol, and drying polyborosiloxane; The diol is heated and mixed in a predetermined device to obtain the first mixed material; the cyclopentane is obtained, and the cyclopentane and the mixed material are placed in an internal mixer for heating and internal mixing to obtain the second mixed material; the second mixed material is obtained; The material is made into flakes, and the flakes are placed in a granulator for granulation to obtain particulate matter; the particulate matter is foamed to obtain high-elasticity nylon.
  • the boron in the polyborosiloxane can interact strongly with oxygen to form physical crosslinking and chemical crosslinking. Compared with the existing nylon elastomer, the Increased permanent compression set rate.
  • FIG. 1 is a flow chart of a method for preparing high-elasticity nylon provided by an embodiment of the present invention.
  • an embodiment of the present invention provides a method for preparing high-elasticity nylon, including:
  • nylon, polyborosiloxane, and polyethylene glycol and dry the polyborosiloxane; wherein, the mass ratio of the nylon to the polyborosiloxane is 10-100:1; The mass of ethylene glycol is 10% of the mass of the polyborosiloxane;
  • nylon, polyborosiloxane, and polyethylene glycol can be directly purchased.
  • the embodiment of the present invention does not specifically limit the purity and content of the above-mentioned components. What needs to be guaranteed is the effective content of each component. It suffices to satisfy the above-mentioned standard that the mass ratio of nylon to polyborosiloxane is 10-100:1; the mass of polyethylene glycol is 10% of the mass of polyborosiloxane.
  • the nylon, the polyborosiloxane, and the polyethylene glycol are placed in a predetermined device for heating and mixing to obtain a first mixed material; wherein the heating temperature is 150-180° C., and the heating time is 3-5 minutes;
  • predetermined equipment can be any equipment that can be heated and can last for a predetermined time, or it can be a heating equipment.
  • the user records the heating time by himself. After the heating is completed, the next process can be directly carried out without cooling.
  • the preparation can also be carried out to the next step after it self-cooling.
  • the quality of the cyclopentane is the quality of the first mixed material 5-10% of the temperature, the mixing temperature is 150-180°C, and the mixing time is 7-10min;
  • the two rotors rotate relative to each other, and the material from the feeding port is clamped and brought into the roll gap to be squeezed and sheared by the rotor. Divided into two parts, respectively along the gap between the front and rear chamber walls and the rotor and then back to the top of the roll gap.
  • the material is subjected to shearing and friction everywhere, so that the temperature of the rubber material rises sharply, the viscosity decreases, and the wettability of the rubber on the surface of the compounding agent is increased, so that the rubber and the compounding agent surface are fully contacted.
  • the batch of compounding agent passes through the gap between the rotor and the rotor, the rotor and the upper and lower top bolts, and the inner wall of the mixer together with the rubber compound. It is sheared and broken, surrounded by the stretched and deformed rubber, and stabilized in a broken state. At the same time, the ridges on the rotor make the rubber material move along the axial direction of the rotor, which plays the role of stirring and mixing, so that the compounding agent is evenly mixed in the rubber material.
  • the compounding agent is repeatedly sheared and broken, the rubber compound repeatedly deforms and recovers, and the rotor ridges are continuously stirred, so that the compounding agent is uniformly dispersed in the compound and reaches a certain degree of dispersion.
  • the cyclopentane and the first mixture are added to the feeding port of the internal mixer, and the internal mixer obtains the second mixture after the above-mentioned processing flow.
  • the second mixed material is formed into flakes and the flakes are granulated in a granulator to obtain a granular material.
  • the method of making the second mixed material into a sheet can be extrusion with a hydraulic press, rolling with a rolling column, or other equipment or methods that can roll objects into thin sheets.
  • the above-mentioned granulator is a molding machine that can make materials into specific shapes.
  • the special screw design and different configurations are adopted, and the reduction box adopts the design of high torque, which realizes the performance of noiseless and stable operation.
  • the screw and barrel are specially hardened, which has the characteristics of wear resistance, good mixing performance and high output.
  • the design of vacuum exhaust or ordinary exhaust port can discharge moisture and waste gas during the production process, so that the material can be discharged. It is more stable and the colloidal particles are stronger, which ensures the good quality of the product.
  • the process of high temperature melting, plasticizing and extrusion is used to change the physical properties of plastics to achieve plasticizing and molding of plastics.
  • the particulate matter is foamed to obtain high elastic nylon; wherein the foaming temperature is 160-180° C., the foaming time is 5-7min, and the foaming pressure is 140-160kg/cm 2 .
  • the equipment used for the above-mentioned foaming is a molding machine or a steam cylinder, and the basic steps of foaming molding are the formation of cell nuclei, the growth or expansion of cell nuclei, and the stabilization of cell nuclei.
  • the solubility of the gas decreases, so that it reaches a saturated state, so that the excess gas is removed and bubbles are formed, thereby achieving nucleation.
  • the foaming temperature is 160-180° C.
  • the foaming time is 5-7 min
  • the foaming pressure is 140-160 kg/cm 2 .
  • the thickness of the sheet is 10mm.
  • the predetermined device is an extruder.
  • the extruder is a twin-screw extruder or a single-screw extruder.
  • the screw extruder relies on the pressure and shear force generated by the rotation of the screw, so that the material can be fully plasticized and uniformly mixed, and formed through the die.
  • a predetermined proportion of nylon, polyborosiloxane and polyethylene glycol are placed at the feed port of the extruder, and under the treatment of the extruder, the above three materials are uniformly mixed. material, that is, the first mixed material.
  • the embodiment of the present invention provides a high-elasticity nylon, which is prepared by the above-mentioned preparation method of the high-elasticity nylon.
  • An embodiment of the present invention provides a method for preparing high-elasticity nylon, including: obtaining nylon, polyborosiloxane, polyethylene glycol, and drying polyborosiloxane; The diol is heated and mixed in a predetermined device to obtain the first mixed material; the cyclopentane is obtained, and the cyclopentane and the mixed material are placed in an internal mixer for heating and internal mixing to obtain the second mixed material; the second mixed material is obtained; The material is made into flakes, and the flakes are placed in a granulator for granulation to obtain particulate matter; the particulate matter is foamed to obtain high-elasticity nylon.
  • the high elastic nylon prepared by the method provided by the embodiment of the present invention greatly improves the permanent compression deformation rate.
  • Step 1 Dry nylon and polyborosiloxane (PBDMS), add them to the extruder in a mass ratio of 10:1, and then add 10% polyethylene glycol-400 by total mass to the extruder, open the The heating module of the extruder is heated, the temperature is 150 °C, and the time is 5 minutes, so that the various materials are mixed evenly;
  • PBDMS polyborosiloxane
  • step 2 the material obtained in step 1 and the foaming agent cyclopentane are put into a Banbury mixer according to the mass ratio of 100:5, and the heating temperature is 150°C, and the banburying time is 10min;
  • Step 3 make the material obtained in step 2 into a 10mm sheet
  • Step 4 the film obtained in step 3 is sent to a granulator for granulation;
  • step 5 the material obtained in step 4 is foamed, the foaming temperature is 160° C., the foaming time is 5 min, and the pressure is 160 kg/cm 2 to obtain high-elasticity nylon.
  • Step 1 Dry nylon and polyborosiloxane (PBDMS), add them to the extruder in a mass ratio of 10:1, and then add 10% polyethylene glycol-400 by total mass to the extruder, open the The heating module of the extruder is heated at a temperature of 180 °C and a time of 3 minutes to mix the various materials evenly;
  • PBDMS polyborosiloxane
  • step 2 the material obtained in step 1 and the blowing agent cyclopentane are put into a Banbury mixer according to a mass ratio of 100:10, and the heating temperature is 180 ° C, and the banburying time is 7min;
  • Step 3 make the material obtained in step 2 into a 10mm sheet
  • Step 4 the film obtained in step 3 is sent to a granulator for granulation;
  • step 5 the material obtained in step 4 is foamed, the foaming temperature is 180° C., the foaming time is 7min, and the pressure is 140kg/cm 2 to obtain high elasticity nylon.
  • Step 1 Dry nylon and polyborosiloxane (PBDMS), add them to the extruder in a mass ratio of 10:1, and then add 10% polyethylene glycol-400 by total mass to the extruder, open the The heating module of the extruder is heated, the temperature is 150 °C, and the time is 5 minutes, so that the various materials are mixed evenly;
  • PBDMS polyborosiloxane
  • step 2 the material obtained in step 1 and the blowing agent cyclopentane are put into a Banbury mixer according to a mass ratio of 100:5, and the heating temperature is 180 ° C, and the banburying time is 7min;
  • Step 3 make the material obtained in step 2 into a 10mm sheet
  • Step 4 the film obtained in step 3 is sent to a granulator for granulation;
  • step 5 the material obtained in step 4 is foamed, the foaming temperature is 170° C., the foaming time is 7min, and the pressure is 140kg/cm 2 to obtain high elasticity nylon.
  • Step 1 Dry nylon and polyborosiloxane (PBDMS), add them to the extruder in a mass ratio of 10:1, and then add 10% polyethylene glycol-400 by total mass to the extruder, open the The heating module of the extruder is heated at a temperature of 180 °C and a time of 3 minutes to mix the various materials evenly;
  • PBDMS polyborosiloxane
  • step 2 the material obtained in step 1 and the foaming agent cyclopentane are put into the internal mixer according to the mass ratio of 100:10, and are heated and mixed in an internal mixer, the heating temperature is 170 ° C, and the internal mixing time is 8min;
  • Step 3 make the material obtained in step 2 into a 10mm sheet
  • Step 4 the film obtained in step 3 is sent to a granulator for granulation;
  • step 5 the material obtained in step 4 is foamed, the foaming temperature is 180° C., the foaming time is 6 min, and the pressure is 140 kg/cm 2 to obtain high-elasticity nylon.
  • Step 1 Dry nylon and polyborosiloxane (PBDMS), add them to the extruder in a mass ratio of 10:1, and then add 10% polyethylene glycol-400 by total mass to the extruder, open the The heating module of the extruder is heated, the temperature is 150 °C, and the time is 5 minutes, so that the various materials are mixed evenly;
  • PBDMS polyborosiloxane
  • step 2 the material obtained in step 1 and the blowing agent cyclopentane are put into a Banbury mixer according to a mass ratio of 100:5, and the heating temperature is 180 ° C, and the banburying time is 7min;
  • Step 3 make the material obtained in step 2 into a 10mm sheet
  • Step 4 the film obtained in step 3 is sent to a granulator for granulation;
  • step 5 the material obtained in step 4 is foamed, the foaming temperature is 170° C., the foaming time is 6 min, and the pressure is 150 kg/cm 2 to obtain high-elasticity nylon.
  • Step 1 Dry nylon and polyborosiloxane (PBDMS), add them to the extruder in a mass ratio of 10:1, and then add 10% polyethylene glycol-400 by total mass to the extruder, open the The heating module of the extruder is heated, the temperature is 150 °C, and the time is 5 minutes, so that the various materials are mixed evenly;
  • PBDMS polyborosiloxane
  • step 2 the material obtained in step 1 and the blowing agent cyclopentane are put into a Banbury mixer according to a mass ratio of 100:5, and the heating temperature is 180 ° C, and the banburying time is 7min;
  • Step 3 make the material obtained in step 2 into a 10mm sheet
  • Step 4 the film obtained in step 3 is sent to a granulator for granulation;
  • step 5 the material obtained in step 4 is foamed, the foaming temperature is 180° C., the foaming time is 5min, and the pressure is 150kg/cm 2 .
  • the compression set test of Examples 2, 3 and the control example is carried out.
  • the test method is that in an environment with a temperature of 70 ° C, the compression deformation is 10%.
  • the compression set rate CS is calculated.
  • the calculation method of CS is:
  • h0 height of sample before compression/mm
  • h1 height of compression deformation/mm
  • h2 height of sample after recovery/mm.
  • the comparison example is made as follows:
  • Step 1 put nylon, polyethylene glycol-400, and cyclopentane into an internal mixer according to the mass ratio of 100:10:5 for heating and banburying, the heating temperature is 150°C, and the banburying time is 10min;
  • Step 2 make the material obtained in step 1 into a 10mm sheet
  • Step 3 the film obtained in step 2 is sent to a granulator for granulation
  • step 4 the material obtained in step 3 is foamed, the foaming temperature is 160° C., the foaming time is 5 min, and the pressure is 160 kg/cm 2 .
  • Example 2 Example 3 Control example Compression Set CS 66.7 60 80

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Emergency Medicine (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Molding Of Porous Articles (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

本发明实施例提供了一种高弹性尼龙的制备方法,包括:获取尼龙、聚硼硅氧烷、聚乙二醇,烘干聚硼硅氧烷;将尼龙、聚硼硅氧烷、聚乙二醇置于预定设备中加热混匀,得到第一混合材料;获取环戊烷,并将环戊烷与混合材料置于密炼机中加热密炼,得到第二混合材料;将第二混合材料制成薄片,并将薄片置于造粒机中造粒,得到颗粒物质;将颗粒物质进行发泡,得到高弹性尼龙。采用本发明实施例提供的方法制备的高弹性尼龙,相较于现有的尼龙弹性体,大大提高了永久压缩变形率。

Description

一种高弹性尼龙及其制备方法 技术领域
本发明涉及尼龙弹性体改性方法技术领域,特别是涉及一种高弹性尼龙及其制备方法。
背景技术
尼龙弹性体(PEBAX)是一种嵌段聚酰胺弹性体产品,属于工程聚合物。该产品既具有相当广泛的硬度范围及良好的回弹性,其显著的加工性能使该产品成为生产部件的理想材料。
尼龙弹性体也具有较好的耐化学品性能、耐热、耐候性能,在运动器材、抗冲击部件、手表外壳等领域得到了广泛地应用。然而,现有的尼龙弹性体的压缩永久变形率较差,受到压缩变形后很难恢复原本的状态。
发明内容
针对现有技术中,现有的尼龙弹性体的压缩永久变形率较差,受到压缩变形后很难恢复原本的状态的技术问题,本发明实施例提供了一种高弹性尼龙及其制备方法。具体技术方案如下:
第一方面,本发明实施例提供了一种高弹性尼龙的制备方法,包括:
获取尼龙、聚硼硅氧烷、聚乙二醇,烘干所述聚硼硅氧烷;其中,所述尼龙与所述聚硼硅氧烷的质量比为10-100:1;所述聚乙二醇的质量为所述聚硼 硅氧烷质量的10%;
将所述尼龙、所述聚硼硅氧烷、所述聚乙二醇置于预定设备中加热混匀,得到第一混合材料;其中加热温度为150-180℃,加热时间为3-5min;
获取环戊烷,并将所述环戊烷与所述混合材料置于密炼机中加热密炼,得到第二混合材料;其中,所述环戊烷的质量为所述第一混合材料质量的5-10%,密炼温度为150-180℃,密炼时间为7-10min;
将所述第二混合材料制成薄片,并将所述薄片置于造粒机中造粒,得到颗粒物质;
将所述颗粒物质进行发泡,得到高弹性尼龙;其中发泡温度为160-180℃,发泡时间为5-7min,发泡压力为140-160kg/cm 2
可选的,所述薄片的厚度为10mm。
可选的,所述预定设备为挤出机。
可选的,所述挤出机为双螺杆挤出机或单螺杆挤出机。
第二方面,本发明实施例提供了一种高弹性尼龙,由上述高弹性尼龙的制备方法制备而成。
本发明实施例提供了一种高弹性尼龙的制备方法,包括:获取尼龙、聚硼硅氧烷、聚乙二醇,烘干聚硼硅氧烷;将尼龙、聚硼硅氧烷、聚乙二醇置于预定设备中加热混匀,得到第一混合材料;获取环戊烷,并将环戊烷与混合材料置于密炼机中加热密炼,得到第二混合材料;将第二混合材料制成薄片,并将薄片置于造粒机中造粒,得到颗粒物质;将颗粒物质进行发泡,得到高弹性尼 龙。采用本发明实施例提供的方法制备的高弹性尼龙,聚硼硅氧烷中的硼可以和氧通过强相互作用,形成物理交联和化学交联,相较于现有的尼龙弹性体,大大提高了永久压缩变形率。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍。
图1是本发明实施例提供的一种高弹性尼龙的制备方法流程图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行描述。
实施例1
请参见图1,第一方面,本发明实施例提供了一种高弹性尼龙的制备方法,包括:
获取尼龙、聚硼硅氧烷、聚乙二醇,烘干所述聚硼硅氧烷;其中,所述尼龙与所述聚硼硅氧烷的质量比为10-100:1;所述聚乙二醇的质量为所述聚硼硅氧烷质量的10%;
需要说明的是,上述尼龙、聚硼硅氧烷、聚乙二醇均可以直接采购获得,本发明实施例不具体限定上述各个成分的纯度以及含量,需要保证的是,各个成分中的有效含量满足上述的尼龙与聚硼硅氧烷的质量比为10-100:1;聚乙二醇的质量为聚硼硅氧烷质量的10%的标准即可。
将所述尼龙、所述聚硼硅氧烷、所述聚乙二醇置于预定设备中加热混匀,得到第一混合材料;其中加热温度为150-180℃,加热时间为3-5min;
需要说明的是,上述预定设备可以是任何可以加温并可以持续预定时间的设备,也可以是一个加热设备,用户自行记录加热时间,加热完成后,无需冷却,便可直接进行下一工序的制备,当然,也可以在其自行冷却后,在进行下一工序。
获取环戊烷,并将所述环戊烷与所述混合材料置于密炼机中加热密炼,得到第二混合材料;其中,所述环戊烷的质量为所述第一混合材料质量的5-10%,密炼温度为150-180℃,密炼时间为7-10min;
需要说明的是,密炼机工作时,两转子相对回转,将来自加料口的物料夹住带入辊缝受到转子的挤压和剪切,穿过辊缝后碰到下顶拴尖棱被分成两部分,分别沿前后室壁与转子之间缝隙再回到辊隙上方。在绕转子流动的一周中,物料处处受到剪切和摩擦作用,使胶料的温度急剧上升,粘度降低,增加了橡胶在配合剂表面的湿润性,使橡胶与配合剂表面充分接触。配合剂团块随胶料一起通过转子与转子间隙、转子与上、下顶拴、密炼室内壁的间隙,受到剪切而破碎,被拉伸变形的橡胶包围,稳定在破碎状态。同时,转子上的凸棱使胶料沿转子的轴向运动,起到搅拌混合作用,使配合剂在胶料中混合均匀。配合剂如此反复剪切破碎,胶料反复产生变形和恢复变形,转子凸棱的不断搅拌,使配合剂在胶料中分散均匀,并达到一定的分散度。由于密炼机混炼时胶料受到的剪切作用比开炼机大得多,炼胶温度高,使得密炼机炼胶的效率大大高于开炼机。具体到本实施例中,将环戊烷与第一混合物加入至密炼机的加料口中, 密炼机经过上述加工流程后,得到第二混合物。
将所述第二混合材料制成薄片,并将所述薄片置于造粒机中造粒,得到颗粒物质。
需要说明的是,将第二混合材料制成薄片的方法可以是利用液压机进行挤压,也可以是利用碾柱进行碾压,还可以是利用其他可以将物体碾压成薄片的设备或方法进行制备;上述造粒机是一种可将物料制造成特定形状的成型机械。采用特殊的螺杆设计及不同配置,减速箱采用高扭矩的设计,实现了无噪音运转平稳等性能。螺杆,料筒经特殊的硬化处理,具有耐磨,混炼性能好,高产量的特性,真空排气或普通排气口的设计,能在生产过程中将水分,废气排走,使出料更稳定,胶粒更结实,保证了产品优良品质。采用高温熔融、塑化、挤出的过程改变塑料的物理性能,达到对塑料的塑化和成型。
将所述颗粒物质进行发泡,得到高弹性尼龙;其中发泡温度为160-180℃,发泡时间为5-7min,发泡压力为140-160kg/cm 2
需要说明的是,上述发泡所使用的设备为成型机或蒸缸,发泡成型的基本步骤是形成泡核、泡核生长或扩大以及泡核的稳定。在给定的温度与压力条件下,气体的溶解度下降,以致达到饱和状态,使多余的气体排除并形成气泡,从而实现成核。具体到本申请中,上述发泡温度为160-180℃,发泡时间为5-7min,发泡压力为140-160kg/cm 2
进一步的,所述薄片的厚度为10mm。
进一步的,所述预定设备为挤出机。
进一步的,所述挤出机为双螺杆挤出机或单螺杆挤出机。
需要说明的是,螺杆挤出机是依靠螺杆旋转产生的压力及剪切力,能使得物料可以充分进行塑化以及均匀混合,通过口模成型。具体到本申请中,将预定比例的尼龙、聚硼硅氧烷、聚乙二醇置于挤出机的入料口,在挤出机的处理下,的带上述三种材料的均匀的混合材料,即第一混合材料。
第二方面,本发明实施例提供了一种高弹性尼龙,由上述高弹性尼龙的制备方法制备而成。
本发明实施例提供了一种高弹性尼龙的制备方法,包括:获取尼龙、聚硼硅氧烷、聚乙二醇,烘干聚硼硅氧烷;将尼龙、聚硼硅氧烷、聚乙二醇置于预定设备中加热混匀,得到第一混合材料;获取环戊烷,并将环戊烷与混合材料置于密炼机中加热密炼,得到第二混合材料;将第二混合材料制成薄片,并将薄片置于造粒机中造粒,得到颗粒物质;将颗粒物质进行发泡,得到高弹性尼龙。采用本发明实施例提供的方法制备的高弹性尼龙,相较于现有的尼龙弹性体,大大提高了永久压缩变形率。
实施例2
在上述实施例1的基础上,本发明实施例以具体实例对本方案做进一步描述。
步骤1,将尼龙、聚硼硅氧烷(PBDMS)烘干,按10:1的质量比例加入挤出机中,再向挤出机中加入总质量10%的聚乙二醇-400,打开挤出机的加热模块进行加热,温度为150℃,时间为5min,使各种材料混合均匀;
步骤2,将步骤1中所得材料与发泡剂环戊烷按照100:5的质量比投入投入密炼机中加热密炼,加热温度为150℃,密炼时间为10min;
步骤3,将步骤2所得材料打成10mm薄片;
步骤4,将步骤3中所得的膜片送入造粒机进行造粒;
步骤5,将步骤4中所得的物料进行发泡,发泡温度为160℃,发泡时间为5min,压力为160kg/cm2,得到高弹性尼龙。
实施例3
步骤1,将尼龙、聚硼硅氧烷(PBDMS)烘干,按10:1的质量比例加入挤出机中,再向挤出机中加入总质量10%的聚乙二醇-400,打开挤出机的加热模块进行加热,温度为180℃,时间为3min,使各种材料混合均匀;
步骤2,将步骤1中所得材料与发泡剂环戊烷按照100:10的质量比投入投入密炼机中加热密炼,加热温度为180℃,密炼时间为7min;
步骤3,将步骤2所得材料打成10mm薄片;
步骤4,将步骤3中所得的膜片送入造粒机进行造粒;
步骤5,将步骤4中所得的物料进行发泡,发泡温度为180℃,发泡时间为7min,压力为140kg/cm2,得到高弹性尼龙。
实施例4
步骤1,将尼龙、聚硼硅氧烷(PBDMS)烘干,按10:1的质量比例加入挤出机中,再向挤出机中加入总质量10%的聚乙二醇-400,打开挤出机的加热模块 进行加热,温度为150℃,时间为5min,使各种材料混合均匀;
步骤2,将步骤1中所得材料与发泡剂环戊烷按照100:5的质量比投入投入密炼机中加热密炼,加热温度为180℃,密炼时间为7min;
步骤3,将步骤2所得材料打成10mm薄片;
步骤4,将步骤3中所得的膜片送入造粒机进行造粒;
步骤5,将步骤4中所得的物料进行发泡,发泡温度为170℃,发泡时间为7min,压力为140kg/cm2,得到高弹性尼龙。
实施例5
步骤1,将尼龙、聚硼硅氧烷(PBDMS)烘干,按10:1的质量比例加入挤出机中,再向挤出机中加入总质量10%的聚乙二醇-400,打开挤出机的加热模块进行加热,温度为180℃,时间为3min,使各种材料混合均匀;
步骤2,将步骤1中所得材料与发泡剂环戊烷按照100:10的质量比投入投入密炼机中加热密炼,加热温度为170℃,密炼时间为8min;
步骤3,将步骤2所得材料打成10mm薄片;
步骤4,将步骤3中所得的膜片送入造粒机进行造粒;
步骤5,将步骤4中所得的物料进行发泡,发泡温度为180℃,发泡时间为6min,压力为140kg/cm2,得到高弹性尼龙。
实施例6
步骤1,将尼龙、聚硼硅氧烷(PBDMS)烘干,按10:1的质量比例加入挤出 机中,再向挤出机中加入总质量10%的聚乙二醇-400,打开挤出机的加热模块进行加热,温度为150℃,时间为5min,使各种材料混合均匀;
步骤2,将步骤1中所得材料与发泡剂环戊烷按照100:5的质量比投入投入密炼机中加热密炼,加热温度为180℃,密炼时间为7min;
步骤3,将步骤2所得材料打成10mm薄片;
步骤4,将步骤3中所得的膜片送入造粒机进行造粒;
步骤5,将步骤4中所得的物料进行发泡,发泡温度为170℃,发泡时间为6min,压力为150kg/cm2,得到高弹性尼龙。
实施例7
步骤1,将尼龙、聚硼硅氧烷(PBDMS)烘干,按10:1的质量比例加入挤出机中,再向挤出机中加入总质量10%的聚乙二醇-400,打开挤出机的加热模块进行加热,温度为150℃,时间为5min,使各种材料混合均匀;
步骤2,将步骤1中所得材料与发泡剂环戊烷按照100:5的质量比投入投入密炼机中加热密炼,加热温度为180℃,密炼时间为7min;
步骤3,将步骤2所得材料打成10mm薄片;
步骤4,将步骤3中所得的膜片送入造粒机进行造粒;
步骤5,将步骤4中所得的物料进行发泡,发泡温度为180℃,发泡时间为5min,压力为150kg/cm2。
试验例
将实施例2、3与对照例进行压缩永久变形测试,测试方法为在温度为70℃的环境中,压缩变形10%,处理24h后,计算压缩永久变形率CS,CS的计算方法为:
CS=(h0-h2)/(h0-h1)
式中,h0:压缩前试样的高度/mm;h1:压缩变形的高度/mm;h2:试样恢复后的高度/mm。
对照例制作方法如下:
步骤1,将尼龙,聚乙二醇-400,环戊烷按照100:10:5的质量比投入密炼机中加热密炼,加热温度为150℃,密炼时间为10min;
步骤2,将步骤1所得材料打成10mm薄片;
步骤3,将步骤2中所得的膜片送入造粒机进行造粒;
步骤4,将步骤3中所得的物料进行发泡,发泡温度为160℃,发泡时间为5min,压力为160kg/cm2。
测试结果如下:
  实施例2 实施例3 对照例
压缩永久变形CS 66.7 60 80
从测试结果中可以发现,实施例2和实施例3相比对照例,其压缩永久变形率CS分别提高了16.7%、25%,说明通过本专利的方法,可以明显提升尼龙弹性体的永久压缩变形率。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将 一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。在没有更多限制的情况下,由语句“包括一个……”限定的要素,并不排除在包括所述要素的过程、方法、物品或者设备中还存在另外的相同要素。
本说明书中的各个实施例均采用相关的方式描述,各个实施例之间相同相似的部分互相参见即可,每个实施例重点说明的都是与其他实施例的不同之处。尤其,对于系统实施例而言,由于其基本相似于方法实施例,所以描述的比较简单,相关之处参见方法实施例的部分说明即可。
以上所述仅为本发明的较佳实施例而已,并非用于限定本发明的保护范围。凡在本发明的精神和原则之内所作的任何修改、等同替换、改进等,均包含在本发明的保护范围内。

Claims (5)

  1. 一种高弹性尼龙的制备方法,其特征在于,包括:
    获取尼龙、聚硼硅氧烷、聚乙二醇,烘干所述聚硼硅氧烷;其中,所述尼龙与所述聚硼硅氧烷的质量比为10-100:1;所述聚乙二醇的质量为所述聚硼硅氧烷质量的10%;
    将所述尼龙、所述聚硼硅氧烷、所述聚乙二醇置于预定设备中加热混匀,得到第一混合材料;其中加热温度为150-180℃,加热时间为3-5min;
    获取环戊烷,并将所述环戊烷与所述混合材料置于密炼机中加热密炼,得到第二混合材料;其中,所述环戊烷的质量为所述第一混合材料质量的5-10%,密炼温度为150-180℃,密炼时间为7-10min;
    将所述第二混合材料制成薄片,并将所述薄片置于造粒机中造粒,得到颗粒物质;
    将所述颗粒物质进行发泡,得到高弹性尼龙;其中发泡温度为160-180℃,发泡时间为5-7min,发泡压力为140-160kg/cm 2
  2. 根据权利要求1所述高弹性尼龙的制备方法,其特征在于,所述薄片的厚度为10mm。
  3. 根据权利要求1所述高弹性尼龙的制备方法,其特征在于,所述预定设备为挤出机。
  4. 根据权利要求3所述高弹性尼龙的制备方法,其特征在于,所述挤出机为双螺杆挤出机或单螺杆挤出机。
  5. 一种高弹性尼龙,由权利要求1-4任一项所述的高弹性尼龙的制备方法制备而成。
PCT/CN2021/097722 2020-07-02 2021-06-01 一种高弹性尼龙及其制备方法 WO2022001557A1 (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2022581719A JP7422252B2 (ja) 2020-07-02 2021-06-01 高弾性ナイロン及びその製造方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN202010632960.5A CN111763418B (zh) 2020-07-02 2020-07-02 一种高弹性尼龙及其制备方法
CN202010632960.5 2020-07-02

Publications (1)

Publication Number Publication Date
WO2022001557A1 true WO2022001557A1 (zh) 2022-01-06

Family

ID=72724508

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2021/097722 WO2022001557A1 (zh) 2020-07-02 2021-06-01 一种高弹性尼龙及其制备方法

Country Status (3)

Country Link
JP (1) JP7422252B2 (zh)
CN (1) CN111763418B (zh)
WO (1) WO2022001557A1 (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115093700A (zh) * 2022-07-04 2022-09-23 华润化学材料科技股份有限公司 一种尼龙弹性体材料及其制备方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111763418B (zh) * 2020-07-02 2022-05-03 西安匹克玄铠新材料有限公司 一种高弹性尼龙及其制备方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019138202A1 (fr) * 2018-01-15 2019-07-18 Arkema France Composition thermoplastique élastomère - silicone
CN110234680A (zh) * 2017-01-31 2019-09-13 玛尔提贝斯股份有限公司 热塑性组合物
CN110818966A (zh) * 2019-11-26 2020-02-21 西安匹克玄铠新材料有限公司 一种聚硼硅氧烷改性橡胶的制备方法
CN110903627A (zh) * 2019-10-30 2020-03-24 晋江兴迅新材料科技有限公司 一种热塑性弹性体共混物超临界发泡材料及其制备方法
CN111763418A (zh) * 2020-07-02 2020-10-13 西安匹克玄铠新材料有限公司 一种高弹性尼龙及其制备方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB0130834D0 (en) 2001-12-22 2002-02-06 Design Blue Ltd Energy absorbing material
US20030175497A1 (en) 2002-02-04 2003-09-18 3M Innovative Properties Company Flame retardant foams, articles including same and methods for the manufacture thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110234680A (zh) * 2017-01-31 2019-09-13 玛尔提贝斯股份有限公司 热塑性组合物
WO2019138202A1 (fr) * 2018-01-15 2019-07-18 Arkema France Composition thermoplastique élastomère - silicone
CN110903627A (zh) * 2019-10-30 2020-03-24 晋江兴迅新材料科技有限公司 一种热塑性弹性体共混物超临界发泡材料及其制备方法
CN110818966A (zh) * 2019-11-26 2020-02-21 西安匹克玄铠新材料有限公司 一种聚硼硅氧烷改性橡胶的制备方法
CN111763418A (zh) * 2020-07-02 2020-10-13 西安匹克玄铠新材料有限公司 一种高弹性尼龙及其制备方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115093700A (zh) * 2022-07-04 2022-09-23 华润化学材料科技股份有限公司 一种尼龙弹性体材料及其制备方法

Also Published As

Publication number Publication date
JP2023533933A (ja) 2023-08-07
JP7422252B2 (ja) 2024-01-25
CN111763418B (zh) 2022-05-03
CN111763418A (zh) 2020-10-13

Similar Documents

Publication Publication Date Title
WO2022001557A1 (zh) 一种高弹性尼龙及其制备方法
KR100340475B1 (ko) 목질합성분및그의제조방법과제조장치,전기목질합성분을사용한목질합성판및그의압출성형방법과성형장치
CN112159564A (zh) 一种低密度、低散发性聚丙烯材料及制备方法
JP2000327792A (ja) 熱可塑性樹脂顆粒物の生成方法
CN105670137A (zh) 一种聚丁烯发泡材料及其制备方法
CN111117028A (zh) 高密度珍珠棉及其制备方法
JPH0638460B2 (ja) 放熱シート
CN108314834B (zh) 一种改性线性低密度聚乙烯材料及其制备方法
CN105820482A (zh) 一种四丙氟橡胶材料及其制备方法
CN112895199B (zh) 一种混炼硅橡胶或硅橡胶复合物切片的生产装置和工艺
CN111793270A (zh) 一种鞋材用止滑剂颗粒及其制备方法
CN108912660A (zh) 高性能改性蒙脱土/热塑性聚氨酯弹性体发泡珠粒及其制备方法
CN110713664A (zh) 一种轮胎硫化胶囊的制备方法
CN214491188U (zh) 一种混炼硅橡胶或硅橡胶复合物切片的生产装置
CN112029200B (zh) 一种低密度热塑性动态硫化橡胶材料及其制备方法和应用
CN112126158A (zh) 一种耐磨抗静电bopp薄膜及其制备方法
CN115466507B (zh) 一种低成本的尼龙弹性体发泡鞋底及其制备方法
EP3719098A1 (en) Process for manufacturing super thermal-conductive graphene capsule
CN114316447B (zh) 一种车用tpv材料及其制备方法和应用
CN115181319B (zh) 一种聚苯醚可发泡微粒的制备方法
CN1483761A (zh) Pvc片板材及其生产工艺
CN117863434A (zh) 一种氟弹性体组合物连续物理发泡制备装置
CN113527869A (zh) 一种碳纳米管改性聚氨酯热塑性硫化胶及其制备方法
CN113444344A (zh) 一种耐高温高韧性全生物基降解塑料及其制备方法
CN116769220A (zh) 一种改善pla材料发泡性能的方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 21831951

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2022581719

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 21831951

Country of ref document: EP

Kind code of ref document: A1