WO2024055630A1 - 一种有机磷腈催化高分子量聚硅氧烷连续生产装置 - Google Patents

一种有机磷腈催化高分子量聚硅氧烷连续生产装置 Download PDF

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WO2024055630A1
WO2024055630A1 PCT/CN2023/096318 CN2023096318W WO2024055630A1 WO 2024055630 A1 WO2024055630 A1 WO 2024055630A1 CN 2023096318 W CN2023096318 W CN 2023096318W WO 2024055630 A1 WO2024055630 A1 WO 2024055630A1
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continuous production
weight polysiloxane
organophosphazene
production device
molecular weight
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PCT/CN2023/096318
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English (en)
French (fr)
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李志波
刘月涛
赵娜
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青岛科技大学
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Publication of WO2024055630A1 publication Critical patent/WO2024055630A1/zh

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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
    • 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
    • B01J19/0053—Details of the reactor
    • B01J19/0066—Stirrers
    • 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
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/06—Preparatory processes
    • C08G77/08—Preparatory processes characterised by the catalysts used

Definitions

  • the invention belongs to the technical field of preparation of organic silicon polymer materials, and particularly relates to a continuous production device of high molecular weight polysiloxane.
  • the Si-O main chain structure of the organic silicon material gives it excellent high-low temperature resistance, radiation resistance, oxidation resistance, weather resistance, hydrophobicity, and physiological inertness. It has been widely used in electronic appliances, chemical industry, metallurgy, and construction. , aerospace, aviation, medical materials and many other fields.
  • Polysiloxane is the base material of silicone. The higher the molecular weight, the greater the viscosity, and the better the mechanical properties.
  • the synthesis of high molecular weight polysiloxane generally uses the anionic ring-opening polymerization process of cyclosiloxane.
  • patent CN102225997A uses a polymerization reactor with a multi-layer paddle stirrer and a scraper to synthesize high molecular weight polysiloxane
  • patent CN101824151A uses an extrusion synthesis method to synthesize high molecular weight polysiloxane
  • patent CN109836582A uses a kneader or double Screw mixers serve as polymerization reactors to prepare high molecular weight polysiloxanes.
  • Patent CN1113923C uses two or more heated SV-type static mixers with gradually increasing diameters to form a continuous polymerization reactor in series to prepare high molecular weight polysiloxane.
  • the continuous production of high molecular weight polysiloxane can be achieved,
  • the reactor itself since the reactor itself has no moving parts, relying solely on the special structure of the unit and fluid movement cannot achieve good mass and heat transfer purposes, especially for systems with high viscosity in the later stages of the reaction.
  • the present invention provides an organophosphazene catalyzed high molecular weight polysiloxane continuous production device.
  • a horizontal reaction device with dual-shaft stirring is used.
  • the diameter of the dual-shafts gradually decreases from the feed port to the discharge port.
  • the corresponding nominal diameter of the blade gradually increases from the feed port to the discharge port.
  • Bi-shaft meshing is used to provide transmission. mass, heat transfer and axial driving force.
  • this device can be used for the continuous production of organophosphazene-catalyzed high-molecular-weight polysiloxane. It has good mass and heat transfer effects, uniform products, narrow molecular weight distribution, and low volatile content.
  • this device can be used as a neutralization and devolatilization reactor for high molecular weight polysiloxane with good effect.
  • This device is also suitable for the mixing process of all high-viscosity, high-elasto-plastic materials, and can be matched with various traditional chemical reactors, such as extrusion, drying, granulation, etc.
  • a first aspect of the present invention provides an organophosphazene catalyzed high molecular weight polysiloxane continuous production device, including: a shell 1. Twin screws 2 and 3 are provided in the shell 1. A plurality of feeding ports 4, 5, 7 and a vacuum interface 6 are provided on the top of the housing 1, and a discharge port 8 is provided on one side of the housing 1.
  • a second aspect of the invention provides a production process using the above-mentioned organophosphazene catalyzed high molecular weight polysiloxane continuous production device, including:
  • the materials are added into the housing 1 through different feeding ports, and reacted under the push of the twin screws. At the same time, move towards the discharge port;
  • the opening and closing of the vacuum interface is controlled according to the process requirements, and the vacuum degree in the housing 1 is adjusted.
  • a third aspect of the present invention provides the application of the above-mentioned device in the production of organic silicon materials.
  • the nominal blade diameter gradually increases from the feed port to the discharge port, and the polymerization reaction system increases with the residence time. , the viscosity increases, and high-viscosity materials correspond to large nominal blade diameters, so this reaction device has excellent mass transfer and heat transfer effects.
  • the obtained products are uniform, with narrow molecular weight distribution and low volatile content. It is especially suitable for large viscosity, Continuous production of high molecular weight polysiloxanes.
  • the continuous polymerization device of the present invention can match the production process of high-molecular-weight polysiloxane catalyzed by highly active organophosphazenes, and can also match various traditional chemical reaction equipment, such as extrusion, Deliming, neutralization, drying, granulation, etc. are easy to promote.
  • the device of the present invention has a simple structure, convenient operation, strong practicability, and is easy to popularize.
  • Figure 1 is a schematic structural diagram of an organophosphazene-catalyzed high molecular weight polysiloxane continuous production device of the present invention.
  • 1 is the shell
  • 2 and 3 are twin screws
  • 4 and 7 are feeding ports
  • 6 is the vacuum interface
  • 8 is the discharge port
  • 9 is the motor.
  • the present invention proposes An organophosphazene-catalyzed high-molecular-weight polysiloxane continuous production device is developed. It adopts a horizontal reaction device with biaxial stirring. The biaxial diameter gradually decreases from the feed port to the discharge port, and the corresponding nominal diameter of the blade is from The feed port gradually increases from the feed port to the discharge port, and biaxial meshing is used to provide mass transfer, heat transfer and axial driving force.
  • the gradually increasing blade diameter corresponds to the gradual increase in the axial viscosity of the system, which is more conducive to mass transfer and heat transfer effects. Therefore, the products obtained by this reaction device are uniform, have narrow molecular weight distribution and low volatile content, and are especially suitable for the continuous production of large viscosity and high molecular weight polysiloxane.
  • this device can be matched with various traditional chemical reaction equipment, such as extrusion, deliming, neutralization, drying, granulation, etc., and is easy to promote.
  • An organophosphazene catalyzed high molecular weight polysiloxane continuous production device A horizontal reaction device with dual-shaft stirring is used. The diameter of the dual-shafts gradually decreases from the feed port to the discharge port. The corresponding nominal diameter of the blade gradually increases from the feed port to the discharge port.
  • the stirring shaft and blades are hollow. , external heating and cooling media can be added, and biaxial meshing is used to provide mass transfer, heat transfer and axial driving force.
  • the present invention is mainly aimed at a continuous polymerization device.
  • the design of simultaneous changes in the biaxial diameter and the nominal blade diameter is to enable better mass transfer and heat transfer of high molecular weight polysiloxane and to make the polymerization more uniform and the product more uniform. Uniform. Because as the reaction proceeds, the viscosity distribution of the product in the axial direction becomes larger and larger, and the increase in blade diameter is more conducive to uniform polymerization and reducing the volatile content.
  • the diameter of the double shaft and the nominal diameter of the blade there are no special restrictions on the diameter of the double shaft and the nominal diameter of the blade. They can be designed according to the production capacity of the production device or according to the size of the reaction equipment shell. Its size is to a certain extent The degree indicates the production capacity of the continuous polymerization device. The larger the nominal diameter of the blade, the greater the production capacity.
  • organophosphazene-catalyzed high-molecular-weight polysiloxane continuous production device of the present invention does not limit the type of polysiloxane and can be applied to all continuous production processes of high-viscosity, high-molecular-weight polysiloxane.
  • organophosphazene-catalyzed high-molecular-weight polysiloxane continuous production device of the present invention is not limited to the type of organophosphazene. It can be one or any number of organophosphazene compounds with high ring-opening activity.
  • the reactor working volume and process residence time are not specifically limited.
  • the diameter of the shell 1 needs to match the nominal diameter of the blade, and the residence time needs to match the rotating speed of the stirring shaft.
  • the biaxial diameter gradually decreases from the feed port to the discharge port, and the biaxial length is not limited and can be determined according to the working volume of the reactor. design.
  • the nominal diameter of the stirring blade gradually increases from the feed port to the discharge port, and the nominal diameter of the blade needs to match the inner diameter of the reactor.
  • the shape of the stirring paddle there is no specific limitation on the shape of the stirring paddle, and any paddle that can provide axial driving force can be used.
  • the production process of high molecular weight polysiloxane is a semi-batch method, which means that after polymerization, there must be a process of neutralization and deboiling. Since the continuous production process of the present invention adopts organophosphazene catalysis, there are few side reactions during the polymerization process, and the content of residual monomers or small molecules in the later period is small. The de-reducing step can be omitted, so it can be applied to the device of the present application for high molecular weight polysilica production. Oxane continuous production.
  • the reactor shell, stirring shaft, and blades are hollow, and external heating and cooling media can be added.
  • the organophosphazene catalyzed high molecular weight polysiloxane continuous production device utilizes Biaxial meshing provides mass transfer, heat transfer and axial driving force to achieve continuous production.
  • the organophosphazene catalyzed high molecular weight polysiloxane continuous production device can be matched with various traditional chemical reactors, such as extrusion, deliming, neutralization, drying, granulation, etc.
  • the viscosity range of the material is: 5-200000 Pa.s.
  • the working temperature is: -50-300°C.
  • the reaction residence time is 0.1 to 5 h.
  • the operating pressure range: -200Pa-1.0MPa.
  • the research of the present invention has found that: unlike traditional batch polymerization reactors, the continuous production device of the present invention has excellent mass transfer and heat transfer effects, and the obtained products are uniform, with narrow molecular weight distribution and low volatile content, and are suitable for large viscosity and high molecular weight applications. Continuous production of polysiloxane.
  • An organophosphazene-catalyzed high-molecular-weight polysiloxane continuous production device including: a casing 1. Twin screws 2, 3 are provided in the casing 1. A plurality of feeding ports 4, 3 are provided on the top of the casing 1. 5, 7 and vacuum interface 6, and a discharge port 8 is provided on one side of the housing 1.
  • Operation method Add cyclosiloxane materials, organophosphazene catalysts, and other additives into the housing 1 from different feeding ports, start the motor, and control the twin-screw speed (the screw speed can be adjusted steplessly, and the screw has a minimum
  • the current maximum speed can reach more than 1000r/min. The higher the speed, the greater the shear force and the greater the output), start the switch of the vacuum interface, adjust the pressure to -200Pa-1.0MPa, and the twin-screw speed
  • the residence time of materials in the reactor is controlled by the degree of vacuum to 0.1 to 5 hours, and the working temperature is controlled to -50-300°C for continuous polymerization and discharge.
  • An organophosphazene-catalyzed high-molecular-weight polysiloxane continuous production device including: a casing 1. Twin screws 2, 3 are provided in the casing 1. A plurality of feeding ports 4, 3 are provided on the top of the casing 1. 5, 7 and vacuum interface 6, and a discharge port 8 is provided on one side of the housing 1.
  • the diameter of the twin shafts gradually decreases from the feed port to the discharge port, and the corresponding nominal blade diameter gradually increases from the feed port to the discharge port.
  • An organophosphazene-catalyzed high-molecular-weight polysiloxane continuous production device including: a casing 1. Twin screws 2, 3 are provided in the casing 1. A plurality of feeding ports 4, 3 are provided on the top of the casing 1. 5, 7 and vacuum interface 6, and a discharge port 8 is provided on one side of the housing 1.
  • the twin screws 2 and 3 are arranged in parallel and the two shafts are meshed.
  • An organophosphazene-catalyzed high-molecular-weight polysiloxane continuous production device including: a casing 1. Twin screws 2, 3 are provided in the casing 1. A plurality of feeding ports 4, 3 are provided on the top of the casing 1. 5, 7 and vacuum interface 6, and a discharge port 8 is provided on one side of the housing 1.
  • Screw 2/3 consists of a stirring shaft and a spirally set blade.
  • An organophosphazene-catalyzed high-molecular-weight polysiloxane continuous production device including: a casing 1. Twin screws 2, 3 are provided in the casing 1. A plurality of feeding ports 4, 3 are provided on the top of the casing 1. 5, 7 and vacuum interface 6, and a discharge port 8 is provided on one side of the housing 1.
  • the blades and stirring shaft are hollow structures filled with heating or cooling medium.
  • An organophosphazene-catalyzed high-molecular-weight polysiloxane continuous production device including: a casing 1. Twin screws 2, 3 are provided in the casing 1. A plurality of feeding ports 4, 3 are provided on the top of the casing 1. 5, 7 and vacuum interface 6, and a discharge port 8 is provided on one side of the housing 1.
  • the interior of the housing 1 is filled with heating or cooling medium.
  • An organophosphazene-catalyzed high-molecular-weight polysiloxane continuous production device including: a casing 1. Twin screws 2, 3 are provided in the casing 1. A plurality of feeding ports 4, 3 are provided on the top of the casing 1. 5, 7 and vacuum interface 6, and a discharge port 8 is provided on one side of the housing 1.
  • the twin screws 2 and 3 are connected to the motor 9 respectively.
  • An organophosphazene-catalyzed high-molecular-weight polysiloxane continuous production device including: a casing 1. Twin screws 2, 3 are provided in the casing 1. A plurality of feeding ports 4, 3 are provided on the top of the casing 1. 5, 7 and vacuum interface 6, and a discharge port 8 is provided on one side of the housing 1.
  • the discharge port is composed of a plurality of cones, and the diameter of the cones gradually decreases from the inside to the outside.

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Abstract

本发明属于有机硅高分子材料制备领域，特别涉及一种有机磷腈催化高分子量聚硅氧烷连续生产装置，包括：采用卧式带双轴搅拌的反应装置，双轴直径从进料口到出料口逐渐减小，相应的桨叶公称直径从进料口到出料口逐渐增大，搅拌轴与桨叶中空，可外加加热与冷却介质，利用双轴啮合提供传质、传热以及轴向推动力。本反应装置具有优异的传质、传热效果，所得产物均一、分子量分布窄，挥发分含量低，尤其适用于有机磷腈催化的大粘度、高分子量聚硅氧烷连续化生产。本生产装置可匹配各类传统的化工反应设备，如挤出、脱灰、中和、干燥、造粒等，普适性强，易于推广。

Description

一种有机磷腈催化高分子量聚硅氧烷连续生产装置 技术领域
本发明属于有机硅高分子材料的制备技术领域，特别涉及一种高分子量聚硅氧烷连续生产装置。
背景技术
公开该背景技术部分的信息仅仅旨在增加对本发明的总体背景的理解，而不必然被视为承认或以任何形式暗示该信息构成已经成为本领域一般技术人员所公知的现有技术。
有机硅材料Si-O主链结构，赋予其优异的耐高-低温性能、耐辐射性、耐氧化性、耐候性、疏水性以及生理惰性等，已广泛应用于电子电器、化工、冶金、建筑、航天、航空、医用材料等众多领域。聚硅氧烷作为有机硅的基体材料，分子量越高，粘度越大，力学性能越好。另外，高分子量的聚硅氧烷合成一般采用环硅氧烷的阴离子开环聚合工艺，聚合过程中产物粘度的增加会导致聚合体系的传质、传热问题，严重影响产物的聚合均一性、分子量分布以及挥发分含量。尤其对于有机磷腈催化体系，因其开环活性高，聚合速率快，体系粘度可在短时间内迅速增大，所以对聚合反应器的传质、传热要求更加苛刻。传统的高分子量聚硅氧烷合成一般采用聚合反应釜，间歇或半间歇操作，以保证反应过程中体系的传质、传热，使产物的分子量分布均一。如专利CN102225997A利用带多层桨叶式搅拌器与刮刀的聚合反应釜合成高分子量的聚硅氧烷，专利CN101824151A利用挤出合成法合成高分子量的聚硅氧烷，专利CN109836582A利用捏合机或者双螺杆混合机作为聚合反应器制备高分子量的聚硅氧烷。上述方法虽能解决高 分子量聚硅氧烷聚合过程中的传质、传热问题，但是属于间歇聚合过程，无法实现连续生产。专利CN1113923C利用2个或2个以上的直径逐渐增加的可加热的SV型静态混合器串联组成连续聚合反应器制备高分子量的聚硅氧烷，虽能实现高分子量聚硅氧烷的连续生产，但由于反应器本身没有运动部件，仅仅依靠单元的特殊结构和流体运动，并不能达到很好的传质、传热目的，尤其对于反应后期高粘度的体系。
发明内容
为了克服上述问题，本发明提供了一种有机磷腈催化高分子量聚硅氧烷连续生产装置。采用卧式带双轴搅拌的反应装置，双轴直径从进料口到出料口逐渐减小，相应的桨叶公称直径从进料口到出料口逐渐增大，利用双轴啮合提供传质、传热以及轴向推动力。本装置作为聚合反应器可适用于有机磷腈催化高分子量聚硅氧烷的连续生产，传质、传热效果好，产物均一，分子量分布窄，挥发分含量低。另外，本装置可作为高分子量聚硅氧烷的中和以及脱挥反应器，效果好。本装置亦适用于所有高粘、高弹塑性物料的混炼过程，可匹配各类传统的化工反应器，如挤出、干燥、造粒等。
为了实现上述目的，本发明采用如下技术方案：
本发明的第一个方面，提供了一种有机磷腈催化高分子量聚硅氧烷连续生产装置，包括：壳体1，所述壳体1内设置有双螺杆2、3，所述壳体1顶部设置有多个加料口4、5、7和真空接口6，所述壳体1一侧设置有出料口8。
本发明的第二个方面，提供了一种采用上述有机磷腈催化高分子量聚硅氧烷连续生产装置进行生产的工艺，包括：
根据工艺要求，物料由不同加料口加入壳体1内，在双螺杆推动下进行反应， 同时，向出料口移动；
生产过程中，根据工艺要求控制真空接口的开闭，调节壳体1内的真空度。
本发明的第三个方面，提供了上述的装置在有机硅材料生产中的应用。
本发明的有益效果
(1)与现有技术相比，本发明的高分子量聚硅氧烷连续生产装置，桨叶公称直径从进料口到出料口逐渐增大，而聚合反应体系随着停留时间的增大，粘度增大，高粘度物料对应于大的桨叶公称直径，所以本反应装置具有优异的传质、传热效果，所得产物均一、分子量分布窄，挥发分含量低，尤其适用于大粘度、高分子量聚硅氧烷的连续化生产。
(2)与现有技术相比，本发明的连续聚合装置可匹配高活性有机磷腈催化的高分子量聚硅氧烷的生产工艺，亦可匹配各类传统的化工反应设备，如挤出、脱灰、中和、干燥、造粒等，易于推广。
(3)本发明装置结构简单、运行方便、实用性强，易于推广。
附图说明
构成本发明的一部分的说明书附图用来提供对本发明的进一步理解，本发明的示例性实施例及其说明用于解释本发明，并不构成对本发明的不当限定。
图1为本发明的一种有机磷腈催化高分子量聚硅氧烷连续生产装置结构示意图。
其中，1为壳体，2、3为双螺杆，4、5、7为加料口，6为真空接口，8为出料口、9电机。
具体实施方式
应该指出，以下详细说明都是示例性的，旨在对本发明提供进一步的说明。 除非另有指明，本发明使用的所有技术和科学术语具有与本发明所属技术领域的普通技术人员通常理解的相同含义。
正如背景技术所介绍的，针对目前大粘度、高分子量聚硅氧烷的间歇聚合反应装置，传质、传热效果不佳，产物不均一，分子量分布大，挥发分含量高等缺点，本发明提出了一种有机磷腈催化高分子量聚硅氧烷连续生产装置，采用卧式带双轴搅拌的反应装置，双轴直径从进料口到出料口逐渐减小，相应的桨叶公称直径从进料口到出料口逐渐增大，利用双轴啮合提供传质、传热以及轴向推动力。逐渐增大的桨叶直径对应于体系轴向粘度的逐渐增大，更有利于传质、传热效果。所以本反应装置所得产物均一、分子量分布窄，挥发分含量低，尤其适用于大粘度、高分子量聚硅氧烷的连续化生产。另外，本装置可匹配各类传统的化工反应设备，如挤出、脱灰、中和、干燥、造粒等，易于推广。
具体如下：
一种有机磷腈催化高分子量聚硅氧烷连续生产装置。采用卧式带双轴搅拌的反应装置，双轴直径从进料口到出料口逐渐减小，相应的桨叶公称直径从进料口到出料口逐渐增大，搅拌轴与桨叶中空，可外加加热与冷却介质，利用双轴啮合提供传质、传热以及轴向推动力。
本发明主要是针对一种连续聚合的装置，双轴直径、桨叶公称直径同时变化的设计是为了使高分子量的聚硅氧烷更好的传质、传热以及使聚合更加均匀，产物更加均一。因为随着反应的进行，产物在轴向上的粘度分布越来越大，而桨叶直径的增大更加有利于聚合均匀，降低挥发分含量。
双轴直径、桨叶公称直径的尺寸并无特殊的限定，可根据生产装置生产能力的大小进行设计，或者可根据反应设备壳体的大小进行设计。它的大小在一定程 度上表示出连续聚合的装置生产能力的大小。桨叶公称直径越大，生产能力越大。
研究发现：本发明的有机磷腈催化高分子量聚硅氧烷连续生产装置，对聚硅氧烷的种类不做限定，可适用于所有大粘度、高分子量聚硅氧烷的连续生产工艺。
研究发现：本发明的有机磷腈催化高分子量聚硅氧烷连续生产装置，对有机磷腈的种类不做限定，可以是具有高开环活性的有机磷腈化合物的一种或者任意几种。
所述有机磷腈催化高分子量聚硅氧烷连续生产装置，反应器工作容积与过程停留时间不做具体限定，壳体1的直径需匹配桨叶公称直径，停留时间需与搅拌轴转速匹配。
在一些实施例中，所述有机磷腈催化高分子量聚硅氧烷连续生产装置，双轴直径从进料口到出料口逐渐减小，双轴长度不做限定，可根据反应器工作容积设计。
在一些实施例中，所述有机磷腈催化高分子量聚硅氧烷连续生产装置，搅拌桨叶公称直径从进料口到出料口逐渐增大，桨叶公称直径与反应器的内径需匹配，对搅拌桨的形状不做具体限定，各种可提供轴向推动力的桨叶均可。
目前，高分子量聚硅氧烷的生产工艺均为半间歇法，就是聚合完之后一定会有中和、脱低沸过程。本发明的连续生产工艺，由于采用有机磷腈催化，聚合过程副反应少，后期残余单体或者小分子含量少，可以省去脱低步骤，所以能适用于本申请的装置进行高分子量聚硅氧烷连续生产。在一些实施例中，所述有机磷腈催化高分子量聚硅氧烷连续生产装置，反应器壳体、搅拌轴与桨叶中空，均可外加加热与冷却介质。
在一些实施例中，所述有机磷腈催化高分子量聚硅氧烷连续生产装置，利用 双轴啮合提供传质、传热以及轴向推动力，以达到连续化生产目的。
在一些实施例中，所述有机磷腈催化高分子量聚硅氧烷连续生产装置，可匹配各类传统的化工反应器，如挤出、脱灰、中和、干燥、造粒等。
在一些实施例中，所述物料的粘度范围为：5-200000Pa.s。
在一些实施例中，所述工作温度为：-50-300℃。
在一些实施例中，所述反应停留时间为0.1～5h。
在一些实施例中，所述操作压力范围：-200Pa-1.0MPa。
本发明研究发现：与传统间歇聚合反应器不同，本发明的连续生产装置，具有优异的传质、传热效果，所得产物均一、分子量分布窄，挥发分含量低，适用于大粘度、高分子量聚硅氧烷的连续化生产。
下面结合具体的实施例，对本发明做进一步的详细说明，应该指出，所述具体实施例是对本发明的解释而不是限定。
实施例1
一种有机磷腈催化高分子量聚硅氧烷连续生产装置，包括：壳体1，所述壳体1内设置有双螺杆2、3，所述壳体1顶部设置有多个加料口4、5、7和真空接口6，所述壳体1一侧设置有出料口8。
运行方法：将环硅氧烷物料、有机磷腈催化剂、其他助剂分别从不同加料口依次加入壳体1内，启动电机，控制双螺杆转速(螺杆速度可无级调节，其螺杆有一个最低转数和最高转数，目前最高转速可达1000r/min以上。转速越高，剪切力越大，产量越大)，启动真空接口的开关，调节压力为-200Pa-1.0MPa，双螺杆转速与真空度控制物料在反应器中的停留时间0.1～5h，控制工作温度-50-300℃连续聚合，出料。
实施例2
一种有机磷腈催化高分子量聚硅氧烷连续生产装置，包括：壳体1，所述壳体1内设置有双螺杆2、3，所述壳体1顶部设置有多个加料口4、5、7和真空接口6，所述壳体1一侧设置有出料口8。
双轴直径从进料口到出料口逐渐减小，相应的桨叶公称直径从进料口到出料口逐渐增大。
实施例3
一种有机磷腈催化高分子量聚硅氧烷连续生产装置，包括：壳体1，所述壳体1内设置有双螺杆2、3，所述壳体1顶部设置有多个加料口4、5、7和真空接口6，所述壳体1一侧设置有出料口8。
所述双螺杆2、3平行设置，双轴啮合。
实施例4
一种有机磷腈催化高分子量聚硅氧烷连续生产装置，包括：壳体1，所述壳体1内设置有双螺杆2、3，所述壳体1顶部设置有多个加料口4、5、7和真空接口6，所述壳体1一侧设置有出料口8。
螺杆2/3由搅拌轴和螺旋设置的桨叶组成。
实施例5
一种有机磷腈催化高分子量聚硅氧烷连续生产装置，包括：壳体1，所述壳体1内设置有双螺杆2、3，所述壳体1顶部设置有多个加料口4、5、7和真空接口6，所述壳体1一侧设置有出料口8。
所述桨叶、搅拌轴为中空结构，内部填充有加热或冷却介质。
实施例6
一种有机磷腈催化高分子量聚硅氧烷连续生产装置，包括：壳体1，所述壳体1内设置有双螺杆2、3，所述壳体1顶部设置有多个加料口4、5、7和真空接口6，所述壳体1一侧设置有出料口8。
所述壳体1内部加填有加热或冷却介质。
实施例7
一种有机磷腈催化高分子量聚硅氧烷连续生产装置，包括：壳体1，所述壳体1内设置有双螺杆2、3，所述壳体1顶部设置有多个加料口4、5、7和真空接口6，所述壳体1一侧设置有出料口8。
所述双螺杆2、3分别与电机9相连。
实施例8
一种有机磷腈催化高分子量聚硅氧烷连续生产装置，包括：壳体1，所述壳体1内设置有双螺杆2、3，所述壳体1顶部设置有多个加料口4、5、7和真空接口6，所述壳体1一侧设置有出料口8。
所述出料口由多个圆锥体组成，所述圆锥体的口径由内到外逐渐缩小。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。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，均应包含在本发明的保护范围之内。

Claims (10)

  1. 一种有机磷腈催化高分子量聚硅氧烷连续生产装置，其特征在于，包括：壳体(1)，所述壳体(1)内设置有双螺杆(2)、(3)，所述壳体(1)顶部设置有多个加料口(4)、(5)、(7)和真空接口(6)，所述壳体(1)一侧设置有出料口(8)。
  2. 如权利要求1所述的有机磷腈催化高分子量聚硅氧烷连续生产装置，其特征在于，双轴直径从进料口到出料口逐渐减小，相应的桨叶公称直径从进料口到出料口逐渐增大。
  3. 如权利要求1所述的有机磷腈催化高分子量聚硅氧烷连续生产装置，其特征在于，所述双螺杆(2)、(3)平行设置，双轴啮合。
  4. 如权利要求1所述的有机磷腈催化高分子量聚硅氧烷连续生产装置，其特征在于，螺杆(2)/(3)由搅拌轴和螺旋设置的桨叶组成。
  5. 如权利要求1所述的有机磷腈催化高分子量聚硅氧烷连续生产装置，其特征在于，所述桨叶、搅拌轴为中空结构，内部填充有加热或冷却介质。
  6. 如权利要求1所述的有机磷腈催化高分子量聚硅氧烷连续生产装置，其特征在于，所述壳体(1)内部加填有加热或冷却介质；
    或，所述双螺杆(2)、(3)分别与电机(9)相连。
  7. 如权利要求1所述的有机磷腈催化高分子量聚硅氧烷连续生产装置，其特征在于，所述出料口由多个圆锥体组成，所述圆锥体的口径由内到外逐渐缩小。
  8. 一种采用权利要求1-7任一项所述有机磷腈催化高分子量聚硅氧烷连续生产装置进行生产的工艺，其特征在于，包括：
    根据工艺要求，物料由不同加料口加入生产装置内，在双螺杆推动下进行反应，同时，向出料口移动；
    生产过程中，根据工艺要求控制真空接口的开闭，调节生产装置内的真空度。
  9. 如权利要求8所述的进行生产的工艺，其特征在于，所述物料的粘度范围为：5-200000Pa.s；
    或，所述工作温度为：-50-300℃；
    或，所述反应停留时间为0.1～5h；
    或，所述操作压力范围：-200Pa-1.0MPa。
  10. 权利要求1-7任一项所述的装置在有机硅材料生产中的应用。
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