WO2020172942A1 - 一种高压直流电缆用聚丙烯基绝缘材料改性装置及方法 - Google Patents

一种高压直流电缆用聚丙烯基绝缘材料改性装置及方法 Download PDF

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WO2020172942A1
WO2020172942A1 PCT/CN2019/080312 CN2019080312W WO2020172942A1 WO 2020172942 A1 WO2020172942 A1 WO 2020172942A1 CN 2019080312 W CN2019080312 W CN 2019080312W WO 2020172942 A1 WO2020172942 A1 WO 2020172942A1
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polypropylene
stirring
organic solvent
reactor
heating
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杜伯学
侯兆豪
李忠磊
李进
许然然
韩晨磊
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Tianjin University
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Tianjin University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules

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  • the invention belongs to the technical field of high-voltage direct current transmission equipment, and specifically relates to a modification device and method of polypropylene-based high-voltage cable insulating materials.
  • high-voltage power transmission technology has achieved world-renowned development.
  • high-voltage DC cables are used in island power transmission, ocean resource development and utilization, urban power grid transformation and upgrading, distributed energy grid-connected power transmission, etc.
  • the development of China has important strategic significance.
  • the widely used cross-linked polyethylene cable has a working temperature of only 70°C and cannot be recycled after reaching its working life.
  • polypropylene-based cable insulation materials that can be recycled and reused have received extensive attention from domestic and foreign researchers and cable manufacturers.
  • Polypropylene material not only has excellent dielectric properties, but also has a higher melting point. The development and application of these two properties will help improve the operating temperature, voltage and line current carrying capacity of polypropylene cables, and the application prospects are huge.
  • the injection and accumulation of space charge in the polymer insulating material of the cable causes local electric field distortion in the insulating medium, accelerates the insulation aging, reduces the dielectric strength, and can cause insulation breakdown in severe cases.
  • the current flowing through the cable under high voltage level is very large, and the heat generated by the core makes the cable run at a higher temperature for a long time.
  • the conductivity of the insulating material at high temperature becomes larger and further aggravates the injection, migration and space charge. Aging of insulation. Therefore, improving the space charge characteristics of insulating materials is of great significance for the safe operation of high-voltage DC cables and large-capacity power transmission.
  • the present invention aims to provide a polypropylene-based insulating material modification device and method for high-voltage DC cables.
  • a polypropylene-based insulating material modification device for high-voltage DC cables including a reactor, a heating device, and a stirring device, as well as a computer control unit and a suction filter recovery device;
  • the computer control unit signally connects the heating device, the stirring device, and the suction recovery device, sends instructions, and then controls the process flow;
  • the heating device is composed of a heating control unit, a thermocouple sensor, a resistance heating wire, and a heat-resistant insulating layer.
  • the heating control unit receives temperature control instructions from the computer control unit, temperature feedback information from the thermocouple sensor, and control resistance.
  • the power supply of the heating wire is on and off, and the thermocouple sensor is located in the reaction kettle, and the resistance heating wire is evenly surrounded by the heat-resistant insulating layer;
  • the suction filtration recovery device is composed of a condensing unit, a vacuum pump, a recovery tank, and a waste gas treatment tank; wherein, the condensing unit is composed of a condensation control unit, a refrigerator, a heat transfer oil, a circulating pump, and a condensing pipe, forming a closed loop circuit; wherein, The waste gas treatment tank contains activated carbon and has an opening; among them, the reaction kettle, the condensation unit, the recovery tank, the vacuum pump, and the waste gas treatment tank are connected in sequence through a hollow pipe.
  • the stirring device is composed of a motor control and drive unit, a motor and a stirring rod; wherein the motor control and drive unit receives a rotational speed control command issued by the computer control unit to drive the motor, and the stirring rod passes through the sealing cover of the reactor.
  • the reaction kettle is composed of an inner liner and a sealing cover.
  • the polypropylene composite base material, organic solvent, and crosslinking agent are fully mixed and reacted in a reaction kettle with pressure resistance, heating and stirring functions to obtain a nano-modified polypropylene-based composite insulating material.
  • the second technical scheme of the present invention is a method for modifying polypropylene-based insulating materials for high-voltage DC cables.
  • the above-mentioned modification device is used to combine the polypropylene composite base material, organic solvent, and crosslinking agent with pressure resistance, heating,
  • the fully mixed and reacted reaction kettle with stirring function obtains the nano-modified polypropylene-based composite insulating material, which specifically includes the following steps:
  • the polypropylene composite base material is made by mixing polypropylene, octavinyl POSS, and antioxidants, wherein polypropylene and octaethylene
  • the mass ratio of alkenyl POSS is 4:1 to 5:1, and the antioxidant accounts for 1% to 5% of the total mass of polypropylene and octavinyl POSS;
  • the heating temperature is selected to be 5-10 degrees Celsius lower than the boiling point of the organic solvent used;
  • Cooling recovery After the temperature in the reactor is cooled down, the suction filtration recovery device is turned on to suction filtration, gasification, and condensation of the organic solvent in the reactor to obtain pure organic solvent and modified polypropylene-based composite insulation. material;
  • the cooling temperature is 20-30 degrees Celsius lower than the boiling point of the organic solvent used.
  • polypropylene includes isotactic polypropylene, syndiotactic polypropylene or a blend of both;
  • Antioxidants include antioxidant 1010, antioxidant 1076, antioxidant 618, antioxidant 626, antioxidant 300, antioxidant 1035, and mixtures thereof.
  • the organic solvent in the step (2) includes toluene (CAS No. 108-88-3, molecular formula is C7H8), xylene (CAS No. 1330-20-7, molecular formula is C8H10), isoamyl acetate (CAS No. 123-92-2, molecular formula is C7H14O2), decalin (CAS No. 91-17-8, chemical formula is C10H18), the volume ratio of its input (calculated by L) is the mass of polypropylene composite base material (according to kg) 5 to 6 times.
  • the stirring speed in the step (3) is set at 30-50 r/min.
  • the crosslinking agent includes dicumyl peroxide (chemical formula is C18H22O2, CAS number is 80-43-3), dibenzoyl peroxide (molecular formula is C14H10O4, CAS number is 94-36- 0), vulcanizing agent double 25 (molecular formula is C16H34O4, CAS number is 78-63-7).
  • the present invention has the following advantages:
  • Nano particles can be uniformly dispersed in the polypropylene-based composite insulating material, and the compatibility between nano and polypropylene is better, and an insulating material for high-voltage DC cables with excellent performance can be prepared.
  • Organic solvents are low in toxicity, are produced in a closed manner, and can be recycled and reused, with excellent economic and environmental benefits.
  • Figure 1 is a flowchart of the modification method of polypropylene-based insulating materials for high-voltage DC cables
  • Figure 2 is a polypropylene-based insulating material modification device for HVDC cables.
  • Attached drawings 1-computer control unit, 2-inner tank, 3-sealed cover, 4-heating control unit, 5-resistance heating wire, 6-thermocouple sensor, 7-heat-resistant insulation layer, 8-motor control and Drive unit, 9-motor, 10-stirring rod, 11-condensation control unit, 12-circulation pump, 13-refrigerator, 14-heat conduction oil, 15-condensation tube, 16-recovery tank, 17-vacuum pump, 18-exhaust gas Processing tank.
  • the cross-linking agent dicumyl oxide which accounts for 1% of the total mass of polypropylene and octavinyl POSS, was put into the reactor, and after stirring for 5 minutes, the stirring and heating device was stopped. After the temperature in the reactor drops to 110 degrees Celsius, the suction filtration recovery device is turned on to suction filtration, gasification, and condensation of the organic solvent in the reactor to obtain pure organic solvents and modified polypropylene-based composite insulating materials.
  • the crosslinking agent dicumyl oxide which accounts for 1.5% of the total mass of polypropylene and octavinyl POSS, was put into the reaction kettle, and after stirring for 5 minutes, the stirring and heating device was stopped. After the temperature in the reactor drops to 90 degrees Celsius, the suction filtration recovery device is turned on to suction filtration, gasification, and condensation recovery of the organic solvent in the reactor to obtain pure organic solvents and modified polypropylene-based composite insulating materials.
  • polypropylene (Hainan Petrochemical, PPH-T03), octavinyl POSS (Zhengzhou Alpha Chemical Co., Ltd.), antioxidant 1010 (Germany BASF) and antioxidant 618 (Germany BASF) are compared by mass to 80:20 : 1.5:1.5
  • isoamyl acetate organic solvent whose volume ratio (in L) accounts for 6 times the mass of the polypropylene composite base material (in Kg) into the reaction kettle.
  • the heating device to raise the temperature of the polypropylene composite base material and the organic solvent in the reactor to 130 degrees Celsius and maintain it.
  • the stirring device Turn on the stirring device to fully dissolve the polypropylene composite base material in the reactor in the organic solvent, and keep the stirring speed constant at 30r/min.
  • the crosslinking agent dibenzoyl peroxide which accounts for 3% of the total mass of polypropylene and octavinyl POSS, was put into the reactor, and after stirring for 6 minutes, the stirring and heating device was stopped. After the temperature in the reactor drops to 120 degrees Celsius, the suction filtration recovery device is turned on to suction filtration, gasification, and condensation recovery of the organic solvent in the reactor to obtain pure organic solvents and modified polypropylene-based composite insulating materials.
  • polypropylene (Hainan Petrochemical, PPH-T03), octavinyl POSS (Zhengzhou Alpha Chemical Co., Ltd.), antioxidant 626 (Germany BASF) and antioxidant 1035 (Germany BASF) are compared by mass ratio of 90:16 : 2.5:2.5 Put into the reaction kettle, and put the isoamyl acetate organic solvent with the volume ratio (in L) accounting for 5 times the mass of the polypropylene composite base material (in Kg) into the reaction kettle. Turn on the heating device to raise the temperature of the polypropylene composite base material and the organic solvent in the reactor to 130 degrees Celsius and maintain it.
  • the stirring device Turn on the stirring device so that the polypropylene composite base material in the reactor is fully dissolved in the organic solvent, and the stirring speed is constant and maintained at 30r/min.
  • the crosslinking agent dibenzoyl peroxide which accounts for 3% of the total mass of polypropylene and octavinyl POSS, was put into the reactor, and after stirring for 6 minutes, the stirring and heating device was stopped. After the temperature in the reactor drops to 120 degrees Celsius, the suction filtration recovery device is turned on to suction filtration, gasification, and condensation recovery of the organic solvent in the reactor to obtain pure organic solvents and modified polypropylene-based composite insulating materials.
  • polypropylene (Hainan Petrochemical, PPH-T03), octavinyl POSS (Zhengzhou Alpha Chemical Co., Ltd.), and antioxidant 300 (BASF, Germany) are put into the reactor at a mass ratio of 80:20:5, and the volume The ratio (calculated by L) of the organic solvent of decalin, which accounts for 6 times the mass of the polypropylene composite base material (calculated by Kg), is put into the reactor. Turn on the heating device to increase the temperature of the polypropylene composite base material and the organic solvent in the reactor at 175 degrees Celsius and maintain it. Turn on the stirring device to fully dissolve the polypropylene composite base material in the reactor in the organic solvent, and keep the stirring speed constant at 30r/min.
  • the present invention uses a set of polypropylene-based insulating material modification device for high-voltage DC cables, which is composed of a computer control unit, a reactor, a heating device, a stirring device and a suction filter recovery device.
  • the computer control unit 1 has a man-machine interactive interface function and a communication function; the man-machine interactive interface function can set material parameters, heating temperature, stirring speed, vacuum filtration air pressure, condensation temperature, etc.); among them, the communication function It can send instructions to the heating device, stirring device, and suction filter recovery device to control the process flow.
  • the reaction kettle is composed of a cylindrical stainless steel liner 2 and a stainless steel sealing cover 3, and has a vacuum tightness and an atmospheric pressure resistance of 10 MPa.
  • the heating device is composed of a heating control unit 4, a thermocouple sensor 6, a resistance heating wire 5, and a heat-resistant insulating layer 7.
  • the heating control unit can receive temperature control instructions issued by the computer control unit 1, and the thermocouple sensor 6
  • the temperature feedback information for controlling the power supply of the resistance heating wire 5 is turned on and off.
  • the thermocouple sensor 6 is located in the reaction kettle, and the resistance heating wire 5 evenly surrounds the reaction kettle and is covered by a heat-resistant insulating layer.
  • the stirring device is composed of a motor control and drive unit 8, a motor 9 and a stirring rod 10; wherein the motor control and drive unit 8 can receive a speed control command issued by the computer control unit 1 to drive the motor 9 and the stirring rod 10.
  • the motor control and drive unit 8 can receive a speed control command issued by the computer control unit 1 to drive the motor 9 and the stirring rod 10.
  • the suction filtration recovery device is composed of a condensing unit, a vacuum pump 17, a recovery tank 16, and a waste gas treatment tank 18.
  • the condensing unit is composed of a condensing control unit 11, a refrigerator 13, a heat transfer oil 14, a circulation 12 pump, and a condensing pipe 15 composition, forming a closed loop; among them, the waste gas treatment tank 18 contains activated carbon and has an opening; among them, the reaction kettle, the condensation unit, the recovery tank, the vacuum pump, and the waste gas treatment tank are connected in sequence by a stainless steel hollow pipe.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Organic Insulating Materials (AREA)

Abstract

本发明公开一种高压直流电缆用聚丙烯基绝缘材料改性装置，包括反应釜、加热装置和搅拌装置、计算机控制单元和抽滤回收装置；所述计算机控制单元信号连接所述加热装置、搅拌装置和抽滤回收装置，发送指令，进而控制工艺流程；其中加热控制单元接收计算机控制单元下达的温度控制指令、热偶传感器的温度反馈信息、控制电阻加热丝的电源通断。还公开了改性方法，首先将聚丙烯复合基料和有机溶剂投入到反应釜中；打开加热装置使反应釜中聚丙烯复合基料和有机溶剂升温并保持；搅拌；将占聚丙烯和八乙烯基POSS总质量的1％～3％的交联剂，投入到反应釜中，搅拌5～10min；降温回收。本发明有机溶剂毒性低，密闭生产，而且可回收循环使用，经济及环境效益优异。

Description

一种高压直流电缆用聚丙烯基绝缘材料改性装置及方法 技术领域
本发明属于高压直流输电装备技术领域，具体讲，涉及一种聚丙烯基高压电缆绝缘材料的改性装置及方法。
背景技术
近年来，高电压输电技术取得了举世瞩目的发展，高压直流电缆作为直流输电技术的关键装备，在海岛送电、海洋资源开发与利用、城市电网改造与升级、分布式能源并网输电等方面的发展具有重要战略意义。目前得到广泛应用的交联聚乙烯电缆，其工作温度仅达到70℃，且达到工作寿命后不可回收利用。近年来，可回收再利用的聚丙烯基电缆绝缘材料，受到国内外研究人员及电缆生产厂商的广泛关注。聚丙烯材料不仅具有优异介电性能，而且有较高的熔点，这两方面性能的开发与应用，有助于提高聚丙烯电缆运行温度及电压和线路载流量，应用前景巨大。
高压直流电场下，一方面电缆聚合物绝缘材料内空间电荷的注入和积聚会在绝缘介质引起局部电场的畸变、加速绝缘老化、降低介电强度，严重时可导致绝缘击穿故障。另一方面，高电压等级下通过电缆的电流很大，线芯产生的热量使电缆长期运行在较高温度下，高温下的绝缘材料的电导率变大进一步加重了空间电荷的注入、迁移和绝缘的老化。因此，改善绝缘材料的空间电荷特性，对于高压直流电缆的安全运行和大容量输电具有重要意义。
近年来，纳米材料迅速发展，纳米材料的尺寸效应及界面效应对纳米复合材料的性能影响重大。目前，改善聚丙烯绝缘材料空间电荷特性的方法，多采用将纳米颗粒直接与聚丙烯基体材料进行简单机械共混改性。但由于纳米颗粒本身易团聚、难均匀分散的特点，尤其在实际工业生产中存在投料量大、无法充分混合的弊端，更易导致聚丙烯纳米复合绝缘材料空间电荷性能劣化。因此，如何提高纳米颗粒在聚丙烯基体材料中的分散性及界面相容性，进而改善高压直流电缆用聚丙烯基绝缘材料空间电荷特性具有重要应用价值。
发明内容
为克服现有技术的不足，本发明旨在提出一种高压直流电缆用聚丙烯基绝缘材料改性装置及方法。
为此，本发明采用的技术方案是：一种高压直流电缆用聚丙烯基绝缘材料改性装置，包括反应釜、加热装置和搅拌装置，还包括计算机控制单元和抽滤回收装置；
其中，所述计算机控制单元信号连接所述加热装置、搅拌装置和抽滤回收装置，发送指令，进而控制工艺流程；
其中，所述加热装置，由加热控制单元、热偶传感器、电阻加热丝、耐热绝缘层组成，其中加热控制单元接收计算机控制单元下达的温度控制指令、热偶传感器的温度反馈信息、控制电阻加热丝的电源通断，其中热偶传感器位于反应釜内，其中电阻加热丝均匀环绕在反应釜外并由耐热绝缘层包覆；
其中，所述抽滤回收装置由冷凝单元、真空泵、回收罐、废气处理罐组成；其中，冷凝单元由冷凝控制单元、制冷机、导热油、循环泵、冷凝管组成，构成闭环回路；其中，废气处理罐内含活性炭，有开口；其中，反应釜、冷凝单元、回收罐、真空泵、废气处理罐通过中空管依次相连。
所述搅拌装置，由电机控制和驱动单元、电动机和搅拌棒组成；其中，电机控制和驱动单元接收计算机控制单元下达的转速控制指令进而驱动电动机，搅拌棒为穿过反应釜密封盖。
所述反应釜，由内胆和密封盖组成。
将聚丙烯复合基料、有机溶剂、交联剂在具有耐压、加热、搅拌功能的反应釜中充分混合、反应得到纳米改性的聚丙烯基复合绝缘材料。
本发明的第二个技术方案是一种高压直流电缆用聚丙烯基绝缘材料改性方法,采用上述改性装置，将聚丙烯复合基料、有机溶剂、交联剂在具有耐压、加热、搅拌功能的反应釜中充分混合、反应得到纳米改性的聚丙烯基复合绝缘材料,具体包括如下步骤:
(1)投料：首先将聚丙烯复合基料和有机溶剂投入到反应釜中；
所述聚丙烯复合基料，由聚丙烯、八乙烯基POSS、抗氧剂混合而成，其中聚丙烯和八乙
烯基POSS质量比例为4:1～5:1，抗氧剂占聚丙烯和八乙烯基POSS总质量的1％～5％；
(2)加热：打开加热装置使反应釜中聚丙烯复合基料和有机溶剂升温并保持；
所述升温温度选择低于所用有机溶剂的沸点5～10摄氏度；
(3)搅拌：打开搅拌装置使反应釜中聚丙烯复合基料充分溶解在有机溶剂中，搅拌速度恒定并保持；
(4)接枝反应：将占聚丙烯和八乙烯基POSS总质量的1％～3％的交联剂，投入到反应釜中，搅拌5～10min后，停止搅拌和加热装置；
(5)降温回收：反应釜内温度降温后，打开抽滤回收装置将反应釜内的有机溶剂抽滤、气化、冷凝回收后，分别得到纯净的有机溶剂和改性的聚丙烯基复合绝缘材料；
所述降温温度为低于所用有机溶剂的沸点20～30摄氏度。
所述步骤(1)中聚丙烯包括等规聚丙烯、间规聚丙烯或两者共混物；
八乙烯基-POSS，其CAS号为69655-76-1，分子方程式为C16H24O12Si8；
抗氧剂，包括抗氧剂1010、抗氧剂1076、抗氧剂618、抗氧剂626、抗氧剂300、抗氧剂1035及其混合物。
所述步骤(2)中有机溶剂，包括甲苯(CAS号为108-88-3，分子式为C7H8)、二甲苯(CAS号为1330-20-7，分子式为C8H10)、乙酸异戊酯(CAS号为123-92-2，分子式为C7H14O2)、十氢化萘(CAS号为91-17-8，化学式为C10H18)，其投入的体积比例(按L计)为聚丙烯复合基料质量(按kg计)的5～6倍。
所述步骤(3)中搅拌速度，设定在30-50r/min。
所述步骤(4)中交联剂包括过氧化二异丙苯(化学式为C18H22O2，CAS号为80-43-3)、过氧化二苯甲酰(分子式为C14H10O4，CAS号为94-36-0)、硫化剂双25(分子式为C16H34O4，CAS号为78-63-7)。
本发明与现有技术相比有如下优点：
(1)纳米颗粒可均匀分散在聚丙烯基复合绝缘材料内，纳米与聚丙烯之间的见面相容性更好，可制备得到性能十分优异的高压直流电缆用绝缘材料。
(2)有机溶剂毒性低，密闭生产，而且可回收循环使用，经济及环境效益优异。
(3)工艺设备容易实现，流程清晰容易控制，生产过程中的温度、转速、气压等参数危险性低，可操作性和可实现性优异。
附图说明
图1为高压直流电缆用聚丙烯基绝缘材料改性方法流程图；
图2为高压直流电缆用聚丙烯基绝缘材料改性装置。
附图表记:1-计算机控制单元，2-内胆,3-密封盖,4-加热控制单元,5-电阻加热丝,6-热偶传感器,7-耐热绝缘层,8-电机控制和驱动单元,9-电动机,10-搅拌棒,11-冷凝控制单元,12-循环泵,13-制冷机,14-导热油,15-冷凝管,16-回收罐,17-真空泵,18-废气处理罐。
具体实施方式：
下面结合实施例及附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例1
首先将聚丙烯(海南石化，PPH-T03)、八乙烯基POSS(郑州阿尔法化工有限公司)、抗氧剂1010(德国BASF巴斯夫)按质量比80：20：1投入到反应釜中，将体积比例(按L计)占聚丙烯复合基料质量(按Kg计)的5倍的二甲苯有机溶剂投入反应釜中。打开加热装置使 反应釜中聚丙烯复合基料和有机溶剂升温125摄氏度并保持。打开搅拌装置使反应釜中聚丙烯复合基料充分溶解在有机溶剂中，搅拌速度恒定30r/min并保持。将占聚丙烯和八乙烯基POSS总质量的1％的交联剂氧化二异丙苯，投入到反应釜中，搅拌5min后，停止搅拌和加热装置。待反应釜内温度降至110摄氏度后，打开抽滤回收装置将反应釜内的有机溶剂抽滤、气化、冷凝回收后，分别得到纯净的有机溶剂和改性的聚丙烯基复合绝缘材料。
实施例2
首先将聚丙烯(海南石化，PPH-T03)、八乙烯基POSS(郑州阿尔法化工有限公司)、抗氧剂1076(德国BASF巴斯夫)按质量比90：16：2投入到反应釜中，将体积比例(按L计)占聚丙烯复合基料质量(按Kg计)的5.5倍的有机溶剂甲苯投入反应釜中。打开加热装置使反应釜中聚丙烯复合基料和有机溶剂升温100摄氏度并保持。打开搅拌装置使反应釜中聚丙烯复合基料充分溶解在有机溶剂中，搅拌速度恒定35r/min并保持。将占聚丙烯和八乙烯基POSS总质量的1.5％的交联剂氧化二异丙苯，投入到反应釜中，搅拌5min后，停止搅拌和加热装置。待反应釜内温度降至90摄氏度后，打开抽滤回收装置将反应釜内的有机溶剂抽滤、气化、冷凝回收后，分别得到纯净的有机溶剂和改性的聚丙烯基复合绝缘材料。
实施例3
首先将聚丙烯(海南石化，PPH-T03)、八乙烯基POSS(郑州阿尔法化工有限公司)、抗氧剂1010(德国BASF巴斯夫)和抗氧剂618(德国BASF巴斯夫)按质量比80：20：1.5：1.5投入到反应釜中，将体积比例(按L计)占聚丙烯复合基料质量(按Kg计)的6倍的乙酸异戊酯有机溶剂投入反应釜中。打开加热装置使反应釜中聚丙烯复合基料和有机溶剂升温130摄氏度并保持。打开搅拌装置使反应釜中聚丙烯复合基料充分溶解在有机溶剂中，搅拌速度恒定30r/min并保持。将占聚丙烯和八乙烯基POSS总质量的3％的交联剂过氧化二苯甲酰，投入到反应釜中，搅拌6min后，停止搅拌和加热装置。待反应釜内温度降至120摄氏度后，打开抽滤回收装置将反应釜内的有机溶剂抽滤、气化、冷凝回收后，分别得到纯净的有机溶剂和改性的聚丙烯基复合绝缘材料。
实施例4
首先将聚丙烯(海南石化，PPH-T03)、八乙烯基POSS(郑州阿尔法化工有限公司)、抗氧剂626(德国BASF巴斯夫)和抗氧剂1035(德国BASF巴斯夫)按质量比90：16：2.5：2.5投入到反应釜中，将体积比例(按L计)占聚丙烯复合基料质量(按Kg计)的5倍的乙酸异戊酯有机溶剂投入反应釜中。打开加热装置使反应釜中聚丙烯复合基料和有机溶剂升温130摄氏度并保持。打开搅拌装置使反应釜中聚丙烯复合基料充分溶解在有机溶剂中，搅拌速度 恒定30r/min并保持。将占聚丙烯和八乙烯基POSS总质量的3％的交联剂过氧化二苯甲酰，投入到反应釜中，搅拌6min后，停止搅拌和加热装置。待反应釜内温度降至120摄氏度后，打开抽滤回收装置将反应釜内的有机溶剂抽滤、气化、冷凝回收后，分别得到纯净的有机溶剂和改性的聚丙烯基复合绝缘材料。
实施例5
首先将聚丙烯(海南石化，PPH-T03)、八乙烯基POSS(郑州阿尔法化工有限公司)、抗氧剂300(德国BASF巴斯夫)按质量比80：20：5投入到反应釜中，将体积比例(按L计)占聚丙烯复合基料质量(按Kg计)的6倍的十氢化萘有机溶剂投入反应釜中。打开加热装置使反应釜中聚丙烯复合基料和有机溶剂升温175摄氏度并保持。打开搅拌装置使反应釜中聚丙烯复合基料充分溶解在有机溶剂中，搅拌速度恒定30r/min并保持。将占聚丙烯和八乙烯基POSS总质量的2％的交联剂硫化剂双25，投入到反应釜中，搅拌6min后，停止搅拌和加热装置。待反应釜内温度降至160摄氏度后，打开抽滤回收装置将反应釜内的有机溶剂抽滤、气化、冷凝回收后，分别得到纯净的有机溶剂和改性的聚丙烯基复合绝缘材料。
本发明的工艺流程，如图1所示。
如图2所示，本发明采用一套高压直流电缆用聚丙烯基绝缘材料改性装置，它由计算机控制单元、反应釜、加热装置、搅拌装置和抽滤回收装置组成。
其中，所述计算机控制单元1，具备人机交互界面功能和通讯功能；其中人机交互界面功能可设置物料参数、加热温度、搅拌速度、真空抽滤气压、冷凝温度等)；其中，通讯功能可向加热装置、搅拌装置、抽滤回收装置发送指令，进而控制工艺流程。
其中，所述反应釜，由圆柱形不锈钢内胆2和不锈钢密封盖3组成，具有可抽真空密闭性和抗大气压10MPa性能。
其中，所述加热装置，由加热控制单元4、热偶传感器6、电阻加热丝5、耐热绝缘层7组成，其中加热控制单元可以接收计算机控制单元1下达的温度控制指令、热偶传感器6的温度反馈信息、控制电阻加热丝5的电源通断，其中热偶传感器6位于反应釜内，其中电阻加热丝5均匀环绕在反应釜外并由耐热绝缘层包覆。
其中，所述搅拌装置，由电机控制和驱动单元8、电动机9和搅拌棒10组成；其中，电机控制和驱动单元8可以接收计算机控制单元1下达的转速控制指令进而驱动电动机9，搅拌棒10为穿过反应釜不锈钢密封盖3。
其中，所述的抽滤回收装置由冷凝单元、真空泵17、回收罐16、废气处理罐18组成；其中，冷凝单元由冷凝控制单元11、制冷机13、导热油14、循环12泵、冷凝管15组成， 构成闭环回路；其中，废气处理罐18内含活性炭，有开口；其中，反应釜、冷凝单元、回收罐、真空泵、废气处理罐通过不锈钢中空管依次相连。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式,都包含在本发明的保护范围之内。

Claims (8)

  1. 一种高压直流电缆用聚丙烯基绝缘材料改性装置，包括反应釜、加热装置和搅拌装置，其特征在于，还包括计算机控制单元和抽滤回收装置；
    其中，所述计算机控制单元信号连接所述加热装置、搅拌装置和抽滤回收装置，发送指令，进而控制工艺流程；
    其中，所述加热装置，由加热控制单元、热偶传感器、电阻加热丝、耐热绝缘层组成，其中加热控制单元接收计算机控制单元下达的温度控制指令、热偶传感器的温度反馈信息、控制电阻加热丝的电源通断，其中热偶传感器位于反应釜内，其中电阻加热丝均匀环绕在反应釜外并由耐热绝缘层包覆；
    其中，所述抽滤回收装置由冷凝单元、真空泵、回收罐、废气处理罐组成；其中，冷凝单元由冷凝控制单元、制冷机、导热油、循环泵、冷凝管组成，构成闭环回路；其中，废气处理罐内含活性炭，有开口；其中，反应釜、冷凝单元、回收罐、真空泵、废气处理罐通过中空管依次相连。
  2. 根据权利要求1所述的高压直流电缆用聚丙烯基绝缘材料改性装置，其特征在于，所述搅拌装置，由电机控制和驱动单元、电动机和搅拌棒组成；其中，电机控制和驱动单元接收计算机控制单元下达的转速控制指令进而驱动电动机，搅拌棒为穿过反应釜密封盖。
  3. 根据权利要求1所述的高压直流电缆用聚丙烯基绝缘材料改性装置，其特征在于，所述反应釜由内胆和密封盖组成。
  4. 一种高压直流电缆用聚丙烯基绝缘材料改性方法,采用权利要求1至3中任一项所述的改性装置，其特征在于,将聚丙烯复合基料、有机溶剂、交联剂在具有耐压、加热、搅拌功能的反应釜中充分混合、反应得到纳米改性的聚丙烯基复合绝缘材料,具体包括如下步骤:
    (1)投料：首先将聚丙烯复合基料和有机溶剂投入到反应釜中；
    所述聚丙烯复合基料，由聚丙烯、八乙烯基POSS、抗氧剂混合而成，其中聚丙烯和八乙烯基POSS质量比例为4:1～5:1，抗氧剂占聚丙烯和八乙烯基POSS总质量的1％～5％；
    (2)加热：打开加热装置使反应釜中聚丙烯复合基料和有机溶剂升温并保持；
    所述升温温度选择低于所用有机溶剂的沸点5～10摄氏度；
    (3)搅拌：打开搅拌装置使反应釜中聚丙烯复合基料充分溶解在有机溶剂中，搅拌速度恒定并保持；
    (4)接枝反应：将占聚丙烯和八乙烯基POSS总质量的1％～3％的交联剂，投入到反应釜中，搅拌5～10min后，停止搅拌和加热装置；
    (5)降温回收：反应釜内温度降温后，打开抽滤回收装置将反应釜内的有机溶剂抽滤、 气化、冷凝回收后，分别得到纯净的有机溶剂和改性的聚丙烯基复合绝缘材料；
    所述降温温度为低于所用有机溶剂的沸点20～30摄氏度。
  5. 根据权利要求1所述的一种高压直流电缆用聚丙烯基绝缘材料改性方法,其特征在于,所述步骤(1)中聚丙烯包括等规聚丙烯、间规聚丙烯或两者共混物；
    八乙烯基-POSS；
    抗氧剂，包括抗氧剂1010、抗氧剂1076、抗氧剂618、抗氧剂626、抗氧剂300、抗氧剂1035及其混合物。
  6. 根据权利要求1所述的一种高压直流电缆用聚丙烯基绝缘材料改性方法,其特征在于,所述步骤(2)中有机溶剂，包括甲苯、二甲苯、乙酸异戊酯(CAS号为123-92-2，分子式为C7H14O2)、十氢化萘，其投入的体积比例(按L计)为聚丙烯复合基料质量(按kg计)的5～6倍。
  7. 根据权利要求1所述的一种高压直流电缆用聚丙烯基绝缘材料改性方法,其特征在于,所述步骤(3)中搅拌速度，设定在30-50r/min。
  8. 根据权利要求1所述的一种高压直流电缆用聚丙烯基绝缘材料改性方法,其特征在于,所述步骤(4)中交联剂包括过氧化二异丙苯、过氧化二苯甲酰、硫化剂双25。
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114883052A (zh) * 2022-06-08 2022-08-09 宝新高分子科技(广州)有限公司 一种提高原料流动性的自交联绝缘电缆加工设备

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6214944B1 (en) * 1999-02-02 2001-04-10 Fina Technology, Inc. Method for pressurizing a propylene polymerization reactor
CN205517763U (zh) * 2016-04-21 2016-08-31 新疆华爱康塑业科技发展有限公司 一种聚乙烯交联制备系统

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6214944B1 (en) * 1999-02-02 2001-04-10 Fina Technology, Inc. Method for pressurizing a propylene polymerization reactor
CN205517763U (zh) * 2016-04-21 2016-08-31 新疆华爱康塑业科技发展有限公司 一种聚乙烯交联制备系统

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114883052A (zh) * 2022-06-08 2022-08-09 宝新高分子科技(广州)有限公司 一种提高原料流动性的自交联绝缘电缆加工设备
CN114883052B (zh) * 2022-06-08 2022-12-27 宝新高分子科技(广州)有限公司 一种提高原料流动性的自交联绝缘电缆加工设备

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