CN111320734B - Method for reducing volatile content in resin - Google Patents

Method for reducing volatile content in resin Download PDF

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CN111320734B
CN111320734B CN201811525002.7A CN201811525002A CN111320734B CN 111320734 B CN111320734 B CN 111320734B CN 201811525002 A CN201811525002 A CN 201811525002A CN 111320734 B CN111320734 B CN 111320734B
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resin
volatile content
pressing rollers
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CN111320734A (en
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张帅
欧秋仁
陈超
李阳
王璐
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Aerospace Research Institute of Materials and Processing Technology
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Abstract

本发明提供一种降低树脂中挥发份含量的方法,方法包括:步骤1、设置多辊组件,所述多辊组件至少包括两个压辊;步骤2、将树脂置于多辊组件的任意一组相邻压辊之间,并控制多辊组件的多个压辊进行滚动,其中,任意压辊的温度低于树脂固化温度;步骤3、按照设定时间测量所述相邻压辊之间的树脂中挥发份含量,在所述挥发份含量达到使用要求之前,根据所述挥发份含量调整所述相邻压辊之间的间距,其中,所述挥发份含量与所述间距呈负相关。本发明所提供的方法简单可行,且挥发份含量去除效率高,所得树脂不影响后续使用,能够解决现有的树脂挥发份含量去除的方法中所存在的技术问题。

Figure 201811525002

The present invention provides a method for reducing volatile content in resin. The method includes: step 1, setting up a multi-roller assembly, the multi-roller assembly including at least two pressing rollers; step 2, placing resin on any one of the multi-roller assemblies group between adjacent pressing rollers, and control multiple pressing rollers of the multi-roll assembly to roll, wherein the temperature of any pressing roller is lower than the resin curing temperature; step 3, measure the distance between the adjacent pressing rollers according to the set time The volatile content in the resin, before the volatile content meets the requirements for use, adjust the spacing between the adjacent pressing rollers according to the volatile content, wherein the volatile content is negatively correlated with the spacing . The method provided by the invention is simple and feasible, and the volatile content removal efficiency is high, the obtained resin does not affect subsequent use, and the technical problems existing in the existing resin volatile content removal method can be solved.

Figure 201811525002

Description

降低树脂中挥发份含量的方法Method for reducing volatile content in resin

技术领域technical field

本发明属于复合材料技术领域,具体涉及一种降低树脂中挥发份含量的方法。The invention belongs to the technical field of composite materials, and in particular relates to a method for reducing volatile content in resin.

背景技术Background technique

树脂(通常指酚醛树脂)中可能存在反应过量的酚类物质,同时在生产过程中为了出料的方便需要混入一定量的溶剂,这是酚醛树脂中挥发份的主要成份,以往带有溶剂的树脂可以直接通过湿法制备预浸料,后续经过烘晾去除掉预浸料中的溶剂。但是随着复合材料技术的发展,由于湿法预浸料的质量稳定性差,同时难以达到环保的要求,湿法制备预浸料的工艺已经逐渐被熔融法制备预浸料所取代。但是市场上的树脂绝大多数仍然含有大量的溶剂,要采用热熔法制备树脂预浸料首先需要解决的问题就是降低树脂中挥发份的含量。目前通常降低树脂挥发份含量的方法是将树脂倒在铁盘中放入真空烘箱中抽真空的方法去除溶剂,目前这种方法存在以下问题:There may be excess phenolic substances in the resin (usually referred to as phenolic resin), and a certain amount of solvent needs to be mixed in the production process for the convenience of discharging. This is the main component of volatile matter in phenolic resin. The resin can directly prepare the prepreg by the wet method, and then the solvent in the prepreg can be removed by drying. However, with the development of composite material technology, due to the poor quality stability of wet prepreg and the difficulty in meeting the requirements of environmental protection, the process of preparing prepreg by wet method has been gradually replaced by the preparation of prepreg by melting method. However, the vast majority of resins on the market still contain a large amount of solvent. To prepare resin prepregs by hot melt method, the first problem to be solved is to reduce the content of volatile matter in the resin. At present, the method of reducing the volatile content of resin is to pour the resin into an iron pan and put it in a vacuum oven to remove the solvent. At present, this method has the following problems:

1)溶剂去除效率低。采用抽真空的方式在前期能较快去除树脂中的溶剂,但随着表层树脂溶剂含量降低,体系粘度增大,表层树脂结皮阻碍底层溶剂往外挥发,导致溶剂去除效率急剧下降;1) The solvent removal efficiency is low. The method of vacuuming can quickly remove the solvent in the resin in the early stage, but as the solvent content of the surface resin decreases, the viscosity of the system increases, and the resin crust on the surface prevents the bottom solvent from volatilizing, resulting in a sharp drop in the solvent removal efficiency;

2)影响树脂后续使用。为了加快溶剂的挥发,抽真空时将烘箱温度设置在 60℃左右,一般脱除时间为16-24h才能够达到热熔法制备树脂预浸料的要求,但是长时间的高温处理使树脂固化度缓慢提高,影响树脂的固化性能。2) Affect the subsequent use of resin. In order to speed up the volatilization of the solvent, the oven temperature is set at about 60 ℃ when vacuuming, and the general removal time is 16-24 hours to meet the requirements of preparing resin prepregs by hot-melt method, but long-term high temperature treatment makes the resin curing degree Increase slowly, affecting the curing properties of the resin.

发明内容SUMMARY OF THE INVENTION

在下文中给出关于本发明的简要概述,以便提供关于本发明的某些方面的基本理解。应当理解,这个概述并不是关于本发明的穷举性概述。它并不是意图确定本发明的关键或重要部分,也不是意图限定本发明的范围。其目的仅仅是以简化的形式给出某些概念,以此作为稍后论述的更详细描述的前序。The following presents a brief summary of the present invention in order to provide a basic understanding of certain aspects of the invention. It should be understood that this summary is not an exhaustive overview of the invention. It is not intended to identify key or essential parts of the invention nor to limit the scope of the invention. Its sole purpose is to present some concepts in a simplified form as a prelude to the more detailed description that is discussed later.

本发明的目的在于克服现有技术中的不足,提供了降低树脂中挥发份含量的方法,本发明所提供的方法简单可行,且挥发份含量去除效率高,所得树脂不影响后续使用,解决现有的树脂挥发份含量去除的方法中所存在的技术问题。The purpose of the present invention is to overcome the deficiencies in the prior art, and provide a method for reducing the volatile content in the resin. The method provided by the present invention is simple and feasible, and the removal efficiency of the volatile content is high, and the obtained resin does not affect subsequent use. Some technical problems exist in the method of removing volatile content of resin.

本发明的技术解决方案为:提供一种降低树脂中挥发份含量的方法,该方法包括以下步骤:The technical solution of the present invention is to provide a method for reducing volatile matter content in resin, the method comprising the following steps:

步骤1、设置多辊组件,所述多辊组件至少包括两个压辊;Step 1. Set up a multi-roller assembly, and the multi-roller assembly includes at least two pressing rollers;

步骤2、将树脂置于多辊组件的任意一组相邻压辊之间,并控制多辊组件的多个压辊进行滚动,其中,任意压辊的温度低于树脂固化温度;Step 2, placing the resin between any group of adjacent pressing rollers of the multi-roller assembly, and controlling the plurality of pressing rollers of the multi-roller assembly to roll, wherein the temperature of any pressing roller is lower than the curing temperature of the resin;

步骤3、按照设定时间测量所述相邻压辊之间的树脂中挥发份含量,在所述挥发份含量达到使用要求之前,根据所述挥发份含量调整所述相邻压辊之间的间距,其中,所述挥发份含量与所述间距呈负相关。Step 3. Measure the volatile content in the resin between the adjacent pressing rollers according to the set time, and adjust the volatile content between the adjacent pressing rollers according to the volatile content before the volatile content meets the requirements for use. distance, wherein the volatile content is negatively correlated with the distance.

进一步地,所述步骤1还包括设置通风设备,所述通风设备用于对所述树脂进行通风。Further, the step 1 further includes setting a ventilation device, and the ventilation device is used to ventilate the resin.

进一步地,任意所述压辊的温度均为30℃+ΔT,其中,ΔT≤20。Further, the temperature of any of the pressing rollers is 30°C+ΔT, wherein ΔT≤20.

进一步地,所述多辊组件包括两个压辊。Further, the multi-roller assembly includes two pressing rollers.

进一步地,所述多辊组件包括三个压辊。Further, the multi-roller assembly includes three pressing rollers.

进一步地,所述包括三个压辊的多辊组件为三压辊研磨机。Further, the multi-roll assembly including three pressure rollers is a three-pressure roller mill.

进一步地,所述设定时间为10-30min。Further, the set time is 10-30min.

进一步地,所述树脂为酚醛树脂。Further, the resin is a phenolic resin.

进一步地,所述树脂挥发份含量在30~40%时,所述相邻压辊的间距为 0.1~0.5mm;所述树脂挥发份含量在20~30%时,所述相邻压辊的间距为 0.5~2.5mm;所述树脂挥发份含量在5~20%时,所述相邻压辊的间距为 2.5~5.0mm。Further, when the volatile content of the resin is 30-40%, the distance between the adjacent pressing rollers is 0.1-0.5 mm; when the volatile content of the resin is 20-30%, the distance between the adjacent pressing rollers is 0.1-0.5 mm. The spacing is 0.5-2.5 mm; when the volatile content of the resin is 5-20%, the spacing between the adjacent pressing rollers is 2.5-5.0 mm.

进一步地,所述步骤3中,所述树脂中挥发份含量的测量方法为:Further, in described step 3, the measuring method of volatile matter content in described resin is:

取出一定量树脂,平摊在测量纸上,测定质量为m1;Take out a certain amount of resin, spread it on the measuring paper, and measure the mass as m1;

将树脂及称量纸放入烘箱中,按照设定温度,加热一定时间后,测定其质量为m2;Put the resin and weighing paper into the oven, and after heating for a certain time according to the set temperature, measure the mass as m2;

所述树脂中挥发份的含量为((m1-m2)/m1)%。The content of volatile matter in the resin is ((m1-m2)/m1)%.

应用上述技术方案,提供一种可低温降低树脂挥发份含量的方法,采用包括至少两个压辊的多辊组件,利用高速转动的压辊使树脂不断在压辊之间被挤压、不断在压辊上形成连续的树脂膜,并根据挥发份含量通过不断调整上述相邻压辊之间的间距,保证去除效率,上述方式使树脂获得了相同接触空气的几率,树脂挥发份含量可以同步降低且效率高。此外,由于压辊温度设置低并且处理时间短,对树脂后续固化性能几乎没有影响。综上,本发明制备方法操作简单,对树脂后续使用影响较小,经济环保,且有很高的挥发份去除效率(挥发份含量降低至低于10%),应用领域广泛。Applying the above technical solution, a method for reducing the volatile content of resin at a low temperature is provided. A multi-roller assembly comprising at least two pressing rollers is used, and the high-speed rotating pressing rollers are used to make the resin continuously squeezed between the pressing rollers and continuously in the resin. A continuous resin film is formed on the pressure roller, and the distance between the adjacent pressure rollers is continuously adjusted according to the volatile content to ensure the removal efficiency. The above method enables the resin to obtain the same probability of contacting the air, and the volatile content of the resin can be simultaneously reduced. and high efficiency. In addition, due to the low temperature setting of the rollers and the short treatment time, there is little impact on the resin post-curing properties. In conclusion, the preparation method of the present invention is simple to operate, has little impact on the subsequent use of the resin, is economical and environmentally friendly, has high volatile content removal efficiency (the volatile content is reduced to less than 10%), and has wide application fields.

附图说明Description of drawings

所包括的附图用来提供对本发明实施例的进一步的理解,其构成了说明书的一部分,用于例示本发明的实施例,并与文字描述一起来阐释本发明的原理。显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention, constitute a part of the specification, are used to illustrate the embodiments of the invention, and together with the description, serve to explain the principles of the invention. Obviously, the drawings in the following description are only some embodiments of the present invention, and for those of ordinary skill in the art, other drawings can also be obtained from these drawings without creative effort.

图1为根据本发明实施例提供的采用两压辊的多辊组件去除树脂挥发份含量的示意图;FIG. 1 is a schematic diagram of removing resin volatile content by a multi-roll assembly using two pressing rollers according to an embodiment of the present invention;

图2为根据本发明实施例提供的采用三压辊的多辊组件去除树脂挥发份含量的示意图。FIG. 2 is a schematic diagram of removing the volatile content of resin by a multi-roll assembly using three pressing rollers according to an embodiment of the present invention.

具体实施方式Detailed ways

下面对本发明的具体实施例进行详细说明。在下面的描述中,出于解释而非限制性的目的,阐述了具体细节,以帮助全面地理解本发明。然而,对本领域技术人员来说显而易见的是,也可以在脱离了这些具体细节的其它实施例中实践本发明。Specific embodiments of the present invention will be described in detail below. In the following description, for purposes of explanation and not limitation, specific details are set forth in order to assist in a comprehensive understanding of the present invention. However, it will be apparent to those skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details.

在此需要说明的是,为了避免因不必要的细节而模糊了本发明,在附图中仅仅示出了与根据本发明的方案密切相关的设备结构和/或处理步骤,而省略了与本发明关系不大的其他细节。It should be noted here that, in order to avoid obscuring the present invention due to unnecessary details, the accompanying drawings only show the device structure and/or processing steps closely related to the solution according to the present invention, and omit the details related to the present invention. Invent other details that are less relevant.

正如背景技术所涉及,现有去除树脂中挥发份含量的方法是倒在铁盘中放入真空烘箱中抽真空的方法去除,该方法一是溶剂去除效率低;二是温度过高影响树脂后续使用。基于该背景,本发明实施例提供一种降低树脂挥发份含量的方法,本发明所提供的方法简单可行,且挥发份含量去除效率高,所得树脂不影响后续使用,解决现有的树脂挥发份含量去除的方法中所存在的技术问题。本发明实施例所提供的一种降低树脂挥发份含量的方法包括以下步骤:As involved in the background art, the existing method for removing the volatile content in the resin is to pour it into an iron pan and put it in a vacuum oven to remove it by vacuuming. The method is that the solvent removal efficiency is low; use. Based on this background, the embodiment of the present invention provides a method for reducing the volatile content of resin. The method provided by the present invention is simple and feasible, and the removal efficiency of volatile content is high, the obtained resin does not affect subsequent use, and solves the problem of existing resin volatiles The technical problems existing in the method of content removal. A method for reducing the volatile content of resin provided by the embodiment of the present invention comprises the following steps:

步骤1、设置多辊组件,所述多辊组件至少包括两个压辊;Step 1. Set up a multi-roller assembly, and the multi-roller assembly includes at least two pressing rollers;

步骤2、将树脂置于多辊组件的任意一组相邻压辊之间,并控制多辊组件的多个压辊进行滚动,其中,任意压辊的温度低于树脂固化温度;Step 2, placing the resin between any group of adjacent pressing rollers of the multi-roller assembly, and controlling the plurality of pressing rollers of the multi-roller assembly to roll, wherein the temperature of any pressing roller is lower than the curing temperature of the resin;

步骤3、按照设定时间测量所述相邻压辊之间的树脂中挥发份含量,在所述挥发份含量达到使用要求之前,根据所述挥发份含量调整所述相邻压辊之间的间距,其中,所述挥发份含量与所述间距呈负相关。Step 3. Measure the volatile content in the resin between the adjacent pressing rollers according to the set time, and adjust the volatile content between the adjacent pressing rollers according to the volatile content before the volatile content meets the requirements for use. distance, wherein the volatile content is negatively correlated with the distance.

本发明实施例中,所述树脂可以为酚醛树脂。In the embodiment of the present invention, the resin may be a phenolic resin.

本发明实施例中,上述多辊组件包括的多个压辊为水平设置的多个压辊,各个压辊应处于同一水平面上,即压辊的最高点切面为同一水平面。In the embodiment of the present invention, the multiple pressure rollers included in the multi-roller assembly are multiple pressure rollers arranged horizontally, and each pressure roller should be on the same horizontal plane, that is, the highest point cutting plane of the pressure rollers is the same horizontal plane.

本发明实施例中,如图1-2所示,任意相邻压辊的滚动方向为相向滚动,例如其中一压辊为逆时针滚动,与其相邻压辊设置为顺时针滚动。此外,关于压辊的控制的具体手段可采用本领域公知技术,在此不再详细赘述。In the embodiment of the present invention, as shown in Figures 1-2, the rolling directions of any adjacent pressure rollers are opposite to each other, for example, one of the pressure rollers rolls counterclockwise, and the adjacent pressure rollers are set to roll clockwise. In addition, the specific means for the control of the pressing roller may adopt the technology known in the art, which will not be described in detail here.

本发明实施例中,置于相邻压辊之间的树脂应不超过任意压辊的最高点。In the embodiment of the present invention, the resin placed between adjacent pressing rolls should not exceed the highest point of any pressing roll.

本发明实施例中,多辊组件的所述相邻压辊是运动相向的两个压辊,如图所示的,第一辊和第二辊,或第二辊和第三辊,此外,除另有说明,本发明实施例所述的相邻压辊是指步骤2中所述的放置树脂的一组相邻压辊。In the embodiment of the present invention, the adjacent pressing rollers of the multi-roller assembly are two pressing rollers that move towards each other, as shown in the figure, the first roller and the second roller, or the second roller and the third roller, in addition, Unless otherwise specified, the adjacent pressing rollers in the embodiments of the present invention refer to a group of adjacent pressing rollers on which the resin is placed as described in step 2.

本发明实施例中,所有相邻压辊之间的初始间距可根据树脂挥发份初始含量确定,例如对于酚醛树脂来说,其所述树脂挥发份初始含量在30~40%,此时设置初始间距为0.1~0.5mm。In the embodiment of the present invention, the initial spacing between all adjacent pressing rollers can be determined according to the initial content of resin volatiles. For example, for phenolic resin, the initial volatile content of the resin is 30-40%. The spacing is 0.1 to 0.5 mm.

本发明实施例提供的一种可低温降低树脂挥发份含量的方法,采用包括至少两个压辊的多辊组件,利用高速转动的压辊使树脂不断在压辊之间被挤压、不断在压辊上形成连续的树脂膜(应当注意,方法过程中,树脂并不是全部粘在压辊上的,树脂会在进入到小的间距处时部分被挤压脱离压辊,由此形成动态的树脂膜),使树脂获得了相同接触空气的几率,树脂挥发份含量可以同步降低且效率高,并根据挥发份含量通过不断调整相邻压辊之间的间距,在保证树脂留存到例如第一辊和第二辊间隙的前提下,尽可能提高压辊表面树脂膜的厚度,增加树脂在辊上成膜的时间,进而保证去除效率。此外,由于压辊温度设置低,对树脂后续固化性能几乎没有影响。The embodiment of the present invention provides a method for reducing the volatile content of resin at a low temperature. A multi-roller assembly including at least two pressing rollers is adopted, and the high-speed rotating pressing rollers are used to make the resin continuously squeezed between the pressing rollers and continuously A continuous resin film is formed on the pressure roll (it should be noted that during the method, the resin is not all adhered to the pressure roll, and the resin will be partially squeezed off the pressure roll when entering a small gap, thereby forming a dynamic resin film), so that the resin has the same probability of contacting the air, the volatile content of the resin can be simultaneously reduced and the efficiency is high, and according to the volatile content, by continuously adjusting the distance between the adjacent pressing rollers, it is ensured that the resin is retained until, for example, the first On the premise of the gap between the roller and the second roller, increase the thickness of the resin film on the surface of the pressure roller as much as possible, increase the time for the resin to form a film on the roller, and then ensure the removal efficiency. In addition, due to the low temperature setting of the rollers, there is little effect on the post-curing properties of the resin.

作为本发明一种实施例,为了进一步提高树脂中挥发份的去除效率,所述步骤1还包括设置通风设备,所述通风设备用于对所述树脂进行通风。通过此种设计方式,通过增加树脂与空气接触面积、并保证树脂获得相同接触空气的几率,在通风和加热情况下,保证了挥发份的去除效率。As an embodiment of the present invention, in order to further improve the removal efficiency of volatile matter in the resin, the step 1 further includes setting a ventilation device, and the ventilation device is used to ventilate the resin. Through this design method, by increasing the contact area between resin and air, and ensuring that the resin has the same probability of contacting air, the removal efficiency of volatiles is ensured under the condition of ventilation and heating.

作为本发明一种实施例,为了保证挥发份的去除效率,且不影响树脂的后续使用,任意所述压辊的温度均为30℃+ΔT,其中,ΔT≤20。由此可见,本发明实施例方法在低温下即可完成去除树脂中挥发份,保证了树脂的后续使用效果。As an embodiment of the present invention, in order to ensure the removal efficiency of volatile matter and not affect the subsequent use of the resin, the temperature of any of the pressing rollers is 30°C+ΔT, where ΔT≤20. It can be seen that the method of the embodiment of the present invention can complete the removal of the volatile matter in the resin at low temperature, which ensures the subsequent use effect of the resin.

作文一种具体实施例,对于酚醛树脂来说,所述的压辊温度可以设置为30 ℃~50℃。As a specific example, for the phenolic resin, the temperature of the pressing roller can be set to 30°C to 50°C.

作为本发明一种实施例,上述多辊组件所包括的压辊不超过三个。一则。压辊过多导致成本增加,二则,树脂基本是在上述相邻压辊上进行挤压、成膜,在后的压辊上树脂含量并不会很多(对应方法中只需调节上述相邻压辊的间距即可)。综合两个因素,优选设置压辊不超过三个。As an embodiment of the present invention, the above-mentioned multi-roller assembly includes no more than three pressing rollers. One of. Too many pressing rollers lead to an increase in cost. Second, the resin is basically extruded and formed into a film on the above-mentioned adjacent pressing rollers, and the resin content on the subsequent pressing rollers is not much (in the corresponding method, it is only necessary to adjust the above-mentioned adjacent pressing rollers). The spacing of the pressing rollers is sufficient). Taking two factors into consideration, it is preferable to set no more than three pressing rollers.

作为一种具体实施例,如图1所示,所述多辊组件包括两个压辊。As a specific embodiment, as shown in FIG. 1 , the multi-roller assembly includes two pressing rollers.

作为一种具体实施例,如图2所示,所述多辊组件包括三个压辊。As a specific embodiment, as shown in FIG. 2 , the multi-roller assembly includes three pressing rollers.

更具体的,所述包括三个压辊的多辊组件可以为三压辊研磨机,三辊研磨机为现有的一个设备,如图2所示,下面对基于三辊研磨机的本发明实施例的方法进行举例说明:More specifically, the multi-roll assembly including three pressure rollers can be a three-roll mill, and the three-roll mill is an existing device, as shown in FIG. The method of the invention embodiment is illustrated by an example:

1:开动三辊研磨机,前辊(第一辊,下同)与第二辊间隙控制在初始间距,刮刀离开后辊(第三辊)辊面,将一定量酚醛酚醛树脂缓慢倾倒于三辊研磨机前辊与第二辊中间,酚醛树脂量以覆盖住间隙,与前辊的最高点平齐为准;1: Start the three-roll mill, control the gap between the front roller (the first roller, the same below) and the second roller at the initial distance, the scraper leaves the roller surface of the rear roller (third roller), and slowly pour a certain amount of phenolic phenolic resin onto the three rollers. Between the front roller and the second roller of the roller mill, the amount of phenolic resin should cover the gap and be flush with the highest point of the front roller;

2:每隔设定时间测试一次树脂挥发份含量,根据挥发份含量调节辊间距;其中,酚醛树脂连续在三辊研磨机上滚动,辊温控制在30-50℃,利用三辊研磨机研磨产生热量使酚醛树脂挥发,同时开动通风设备,加快空气流动速度;2: Test the volatile content of the resin every set time, and adjust the roller spacing according to the volatile content; among them, the phenolic resin is continuously rolled on the three-roll mill, and the roller temperature is controlled at 30-50 ° C, and the three-roll mill is used to grind the resulting The heat volatilizes the phenolic resin, and at the same time, the ventilation equipment is activated to speed up the air flow;

3:酚醛树脂挥发份达到要求以后,将刮刀贴合后辊,将酚醛树脂从三辊研磨机上刮下,流到收集装置中。3: After the volatile content of the phenolic resin meets the requirements, the scraper is attached to the rear roller, and the phenolic resin is scraped off the three-roller mill and flows into the collecting device.

作为本发明一种实施例,所述设定时间可以为10-30min,还可以为 20-30min。As an embodiment of the present invention, the set time may be 10-30 min, or 20-30 min.

作为本发明一种实施例,为了提高树脂中挥发份的去除效率,树脂中挥发份含量与相邻压辊的间距可以设置为具有如下关系:所述树脂挥发份含量在 30~40%时,所述相邻压辊的间距为0.1~0.5mm;所述树脂挥发份含量在20~30%时,所述相邻压辊的间距为0.5~2.5mm;所述树脂挥发份含量在5~20%时,所述相邻压辊的间距为2.5~5.0mm。通过此种配置方式,在上述挥发份含量和相邻压辊间距特定关系下,可以保证挥发份含量的去除效率达到最优。As an embodiment of the present invention, in order to improve the removal efficiency of volatile matter in the resin, the volatile matter content in the resin and the distance between adjacent pressing rollers can be set to have the following relationship: when the volatile matter content of the resin is 30-40%, The distance between the adjacent pressing rollers is 0.1-0.5 mm; when the volatile content of the resin is 20-30%, the distance between the adjacent pressing rollers is 0.5-2.5 mm; the volatile content of the resin is 5-2.5 mm. At 20%, the distance between the adjacent pressing rollers is 2.5-5.0 mm. Through this configuration, under the specific relationship between the above-mentioned volatile content and the distance between adjacent pressing rollers, the removal efficiency of the volatile content can be ensured to be optimal.

作为本发明一种实施例,为了准确获取步骤3中的树脂挥发份的含量,所述步骤3中,所述树脂中挥发份含量的测量方法可以为:As an embodiment of the present invention, in order to accurately obtain the content of the volatile matter of the resin in step 3, in the step 3, the measurement method of the volatile matter content in the resin may be:

取出一定量树脂,平摊在测量纸上,测定质量为m1;Take out a certain amount of resin, spread it on the measuring paper, and measure the mass as m1;

将树脂及称量纸放入烘箱中,按照设定温度,加热一定时间后,测定其质量为m2;Put the resin and weighing paper into the oven, and after heating for a certain time according to the set temperature, measure the mass as m2;

所述树脂中挥发份的含量为((m1-m2)/m1)%。The content of volatile matter in the resin is ((m1-m2)/m1)%.

综上,本发明实施例方法利用高速转动的压辊使树脂不断在压辊之间被挤压,压辊的滚动使其表面形成连续的树脂膜,并根据树脂挥发份含量调节辊间距,以及在树脂膜底部的辊温和上方的空气流动的综合作用下,经过一定的时间,可以实现在较低的温度将酚醛树脂中挥发份含量由40%降低至10%以下。该方法不需要专门溶剂去除装置,适合于粗脱溶剂,具有低温、高效、对酚醛树脂后续固化性能几乎没有影响的优势。该可广泛应用于国防工业、军事、航天及建筑等领域。To sum up, the method of the embodiment of the present invention utilizes high-speed rotating pressure rollers to continuously squeeze the resin between the pressure rollers, the rolling of the pressure rollers forms a continuous resin film on the surface, and adjusts the distance between the rollers according to the volatile content of the resin, and Under the combined effect of the roller at the bottom of the resin film and the air flow above, after a certain period of time, the volatile content in the phenolic resin can be reduced from 40% to less than 10% at a lower temperature. The method does not require a special solvent removal device, is suitable for rough solvent removal, and has the advantages of low temperature, high efficiency, and little effect on the subsequent curing performance of the phenolic resin. It can be widely used in defense industry, military, aerospace and construction and other fields.

以下结合具体实施例对本发明作进一步详细描述,这些实施例不能理解为限制本发明所要求保护的范围。The present invention will be further described in detail below with reference to specific embodiments, which should not be construed as limiting the scope of the claimed protection of the present invention.

下述实施例以酚醛树脂为例,并且设置多辊组件包括三个压辊,具体可采用三辊研磨机。The following examples take phenolic resin as an example, and the multi-roll assembly is set to include three pressing rolls, and specifically, a three-roll mill can be used.

实施例1Example 1

步骤1:开动三辊研磨机,前辊与第二辊间隙控制在0.1mm,刮刀离开后辊辊面,将一定量酚醛酚醛树脂缓慢倾倒于三辊研磨机前辊与第二辊中间,酚醛树脂量以覆盖住间隙,与前辊的最高点平齐为准;Step 1: Start the three-roll mill, the gap between the front roller and the second roller is controlled at 0.1mm, the scraper leaves the surface of the rear roller, and a certain amount of phenolic phenolic resin is slowly poured into the middle of the front roller and the second roller of the three-roller mill. The amount of resin is to cover the gap and be flush with the highest point of the front roller;

步骤2:每隔30min测试一次树脂挥发份含量,根据挥发份含量调节辊间距。酚醛树脂中挥发份含量的测试方法为取出10~20g酚醛树脂,平摊在测量纸上,测定质量为m1。将树脂和称量纸放入烘箱中,温度设定为100℃,10分钟后取出,测定其质量为m2。树脂中挥发份的含量为(m1-m2)/m1%。树脂挥发份含量在30~40%时,辊间距为0.1mm;树脂挥发份含量在20~30%时,辊间距为 0.5mm;树脂挥发份含量在10~20%时,辊间距为2.5mm,其中酚醛树脂连续在三辊研磨机上滚动,辊温控制在30℃,利用三辊研磨机研磨产生热量使酚醛树脂挥发,同时开动通风设备,加快空气流动速度;Step 2: Test the volatile content of the resin every 30 minutes, and adjust the roller spacing according to the volatile content. The test method for the volatile content in the phenolic resin is to take out 10-20 g of the phenolic resin, spread it flat on the measuring paper, and measure the mass as m1. Put the resin and weighing paper into an oven, set the temperature to 100°C, take it out after 10 minutes, and measure its mass as m2. The content of volatile matter in the resin is (m1-m2)/m1%. When the resin volatile content is 30-40%, the roller spacing is 0.1mm; when the resin volatile content is 20-30%, the roller spacing is 0.5mm; when the resin volatile content is 10-20%, the roller spacing is 2.5mm , in which the phenolic resin is continuously rolled on the three-roll mill, and the roller temperature is controlled at 30 ° C. The three-roll mill is used to grind to generate heat to volatilize the phenolic resin, and at the same time, the ventilation equipment is activated to speed up the air flow;

步骤3:酚醛树脂挥发份达到要求以后,将刮刀贴合后辊,将酚醛树脂从三辊研磨机上刮下,流到收集装置中。Step 3: After the volatile content of the phenolic resin meets the requirements, the scraper is attached to the rear roller, and the phenolic resin is scraped off the three-roller mill and flows into the collecting device.

采用本实施例酚醛树脂凝胶时间、树脂挥发份含量由40%降至10%的处理时间及生产效率对比见表1。Table 1 shows a comparison of the gel time of the phenolic resin in this embodiment, the treatment time of the resin volatile content from 40% to 10%, and the production efficiency.

实施例2Example 2

步骤1:开动三辊研磨机,前辊与第二辊间隙控制在0.1mm,刮刀离开后辊辊面,将一定量酚醛酚醛树脂缓慢倾倒于三辊研磨机前辊与第二辊中间,酚醛树脂量以覆盖住间隙,与前辊的最高点平齐为准;Step 1: Start the three-roll mill, the gap between the front roller and the second roller is controlled at 0.1mm, the scraper leaves the surface of the rear roller, and a certain amount of phenolic phenolic resin is slowly poured into the middle of the front roller and the second roller of the three-roller mill. The amount of resin is to cover the gap and be flush with the highest point of the front roller;

步骤2:每隔30min测试一次树脂挥发份含量,根据挥发份含量调节辊间距。酚醛树脂中挥发份含量的测试方法为取出10~20g酚醛树脂,平摊在测量纸上,测定质量为m1。将树脂和称量纸放入烘箱中,温度设定为100℃,10分钟后取出,测定其质量为m2。树脂中挥发份的含量为(m1-m2)/m1%。树脂挥发份含量在30~40%时,辊间距为0.1mm;树脂挥发份含量在20~30%时,辊间距为 0.5mm;树脂挥发份含量在10~20%时,辊间距为2.5mm,其中酚醛树脂连续在三辊研磨机上滚动,辊温控制在40℃,利用三辊研磨机研磨产生热量使酚醛树脂挥发,同时开动通风设备,加快空气流动速度;Step 2: Test the volatile content of the resin every 30 minutes, and adjust the roller spacing according to the volatile content. The test method for the volatile content in the phenolic resin is to take out 10-20 g of the phenolic resin, spread it flat on the measuring paper, and measure the mass as m1. Put the resin and weighing paper into an oven, set the temperature to 100°C, take it out after 10 minutes, and measure its mass as m2. The content of volatile matter in the resin is (m1-m2)/m1%. When the resin volatile content is 30-40%, the roller spacing is 0.1mm; when the resin volatile content is 20-30%, the roller spacing is 0.5mm; when the resin volatile content is 10-20%, the roller spacing is 2.5mm , in which the phenolic resin is continuously rolled on the three-roll mill, and the roller temperature is controlled at 40 ° C. The three-roll mill is used to grind to generate heat to volatilize the phenolic resin, and at the same time, the ventilation equipment is turned on to speed up the air flow;

步骤3:酚醛树脂挥发份达到要求以后,将刮刀贴合后辊,将酚醛树脂从三辊研磨机上刮下,流到收集装置中。Step 3: After the volatile content of the phenolic resin meets the requirements, the scraper is attached to the rear roller, and the phenolic resin is scraped off the three-roller mill and flows into the collecting device.

采用本实施例酚醛树脂凝胶时间、树脂挥发份含量由40%降至10%的处理时间及生产效率对比见表1。Table 1 shows a comparison of the gel time of the phenolic resin in this embodiment, the treatment time of the resin volatile content from 40% to 10%, and the production efficiency.

实施例3Example 3

步骤1:开动三辊研磨机,前辊与第二辊间隙控制在0.1mm,刮刀离开后辊辊面,将一定量酚醛酚醛树脂缓慢倾倒于三辊研磨机前辊与第二辊中间,酚醛树脂量以覆盖住间隙,与前辊的最高点平齐为准;Step 1: Start the three-roll mill, the gap between the front roller and the second roller is controlled at 0.1mm, the scraper leaves the surface of the rear roller, and a certain amount of phenolic phenolic resin is slowly poured into the middle of the front roller and the second roller of the three-roller mill. The amount of resin is to cover the gap and be flush with the highest point of the front roller;

步骤2:每隔30min测试一次树脂挥发份含量,根据挥发份含量调节辊间距。酚醛树脂中挥发份含量的测试方法为取出10~20g酚醛树脂,平摊在测量纸上,测定质量为m1。将树脂和称量纸放入烘箱中,温度设定为100℃,10分钟后取出,测定其质量为m2。树脂中挥发份的含量为(m1-m2)/m1%。树脂挥发份含量在30~40%时,辊间距为0.1mm;树脂挥发份含量在20~30%时,辊间距为 0.5mm;树脂挥发份含量在10~20%时,辊间距为2.5mm,其中酚醛树脂连续在三辊研磨机上滚动,辊温控制在50℃,利用三辊研磨机研磨产生热量使酚醛树脂挥发,同时开动通风设备,加快空气流动速度;Step 2: Test the volatile content of the resin every 30 minutes, and adjust the roller spacing according to the volatile content. The test method for the volatile content in the phenolic resin is to take out 10-20 g of the phenolic resin, spread it flat on the measuring paper, and measure the mass as m1. Put the resin and weighing paper into an oven, set the temperature to 100°C, take it out after 10 minutes, and measure its mass as m2. The content of volatile matter in the resin is (m1-m2)/m1%. When the resin volatile content is 30-40%, the roller spacing is 0.1mm; when the resin volatile content is 20-30%, the roller spacing is 0.5mm; when the resin volatile content is 10-20%, the roller spacing is 2.5mm , in which the phenolic resin is continuously rolled on the three-roll mill, and the roller temperature is controlled at 50 ° C. The three-roll mill is used to grind to generate heat to volatilize the phenolic resin, and at the same time, the ventilation equipment is activated to speed up the air flow;

步骤3:酚醛树脂挥发份达到要求以后,将刮刀贴合后辊,将酚醛树脂从三辊研磨机上刮下,流到收集装置中。Step 3: After the volatile content of the phenolic resin meets the requirements, the scraper is attached to the rear roller, and the phenolic resin is scraped off the three-roller mill and flows into the collecting device.

采用本实施例酚醛树脂凝胶时间、树脂挥发份含量由40%降至10%的处理时间及生产效率对比见表1。Table 1 shows a comparison of the gel time of the phenolic resin in this embodiment, the treatment time of the resin volatile content from 40% to 10%, and the production efficiency.

实施例4Example 4

步骤1:开动三辊研磨机,前辊与第二辊间隙控制在0.5mm,刮刀离开后辊辊面,将一定量酚醛酚醛树脂缓慢倾倒于三辊研磨机前辊与第二辊中间,酚醛树脂量以覆盖住间隙,与前辊的最高点平齐为准;Step 1: Start the three-roll mill, the gap between the front roller and the second roller is controlled at 0.5mm, the scraper leaves the surface of the rear roller, and a certain amount of phenolic phenolic resin is slowly poured into the middle of the front roller and the second roller of the three-roller mill. The amount of resin is to cover the gap and be flush with the highest point of the front roller;

步骤2:每隔30min测试一次树脂挥发份含量,根据挥发份含量调节辊间距。酚醛树脂中挥发份含量的测试方法为取出10~20g酚醛树脂,平摊在测量纸上,测定质量为m1。将树脂和称量纸放入烘箱中,温度设定为100℃,10分钟后取出,测定其质量为m2。树脂中挥发份的含量为(m1-m2)/m1%。树脂挥发份含量在30~40%时,辊间距为0.5mm;树脂挥发份含量在20~30%时,辊间距为 2.5mm;树脂挥发份含量在10~20%时,辊间距为5.0mm,其中酚醛树脂连续在三辊研磨机上滚动,辊温控制在50℃,利用三辊研磨机研磨产生热量使酚醛树脂挥发,同时开动通风设备,加快空气流动速度;Step 2: Test the volatile content of the resin every 30 minutes, and adjust the roller spacing according to the volatile content. The test method for the volatile content in the phenolic resin is to take out 10-20 g of the phenolic resin, spread it flat on the measuring paper, and measure the mass as m1. Put the resin and weighing paper into an oven, set the temperature to 100°C, take it out after 10 minutes, and measure its mass as m2. The content of volatile matter in the resin is (m1-m2)/m1%. When the resin volatile content is 30-40%, the roller spacing is 0.5mm; when the resin volatile content is 20-30%, the roller spacing is 2.5mm; when the resin volatile content is 10-20%, the roller spacing is 5.0mm , in which the phenolic resin is continuously rolled on the three-roll mill, and the roller temperature is controlled at 50 ° C. The three-roll mill is used to grind to generate heat to volatilize the phenolic resin, and at the same time, the ventilation equipment is activated to speed up the air flow;

步骤3:酚醛树脂挥发份达到要求以后,将刮刀贴合后辊,将酚醛树脂从三辊研磨机上刮下,流到收集装置中。Step 3: After the volatile content of the phenolic resin meets the requirements, the scraper is attached to the rear roller, and the phenolic resin is scraped off the three-roller mill and flows into the collecting device.

采用本实施例酚醛树脂凝胶时间、树脂挥发份含量由40%降至10%的处理时间及生产效率对比见表1。Table 1 shows a comparison of the gel time of the phenolic resin in this embodiment, the treatment time of the resin volatile content from 40% to 10%, and the production efficiency.

对比例Comparative ratio

将2Kg酚醛酚醛树脂放入真空烘箱中,温度设置为80℃,经过6h后取出,测得酚醛树脂挥发份含量为25%,120℃凝胶时间为7min,生产效率为0.5kg/h。Put 2Kg of phenolic phenolic resin into a vacuum oven, set the temperature to 80°C, and take it out after 6 hours. The volatile content of the phenolic resin was measured to be 25%, the gel time at 120°C was 7min, and the production efficiency was 0.5kg/h.

表1各实施例测试结果Table 1 Test results of each embodiment

Figure BDA0001904219070000121
Figure BDA0001904219070000121

从表1中可以看出三辊研磨机的辊温越高、辊间隙越大酚醛树脂挥发份去除效率更高,辊温升高后酚醛树脂凝胶时间有所降低,但是对使用没有影响。表中生产效率的是由单位时间内将挥发份含量降低至10%以下的酚醛树脂量。当三辊研磨机的辊径和长度一定时,生产效率取决于辊间隙和辊温度,辊间隙越大,温度越高,生产效率越高。It can be seen from Table 1 that the higher the roll temperature and the larger the roll gap of the three-roll mill, the higher the removal efficiency of phenolic resin volatiles. The gel time of phenolic resin decreases after the roll temperature rises, but it has no effect on the use. The production efficiency in the table is the amount of phenolic resin that reduces the volatile content to 10% or less per unit time. When the roll diameter and length of the three-roll mill are constant, the production efficiency depends on the roll gap and roll temperature. The larger the roll gap and the higher the temperature, the higher the production efficiency.

从表1和对比例可以看出,经过6h处理对比例树脂的挥发份含量较高,生产效率低于本发明,并且树脂凝胶时间明显缩短,表明树脂的固化性能已经受到处理工艺过程的影响,影响后续树脂的使用。As can be seen from Table 1 and the comparative example, the volatile content of the resin of the comparative example is higher after 6h treatment, the production efficiency is lower than that of the present invention, and the resin gel time is significantly shortened, indicating that the curing performance of the resin has been affected by the treatment process. , affecting the use of subsequent resins.

如上针对一种实施例描述和/或示出的特征可以以相同或类似的方式在一个或更多个其它实施例中使用,和/或与其它实施例中的特征相结合或替代其它实施例中的特征使用。Features described and/or illustrated above for one embodiment may be used in the same or similar manner in one or more other embodiments, and/or in combination with or instead of features in other embodiments Features in use.

应该强调,术语“包括/包含”在本文使用时指特征、整件、步骤或组件的存在,但并不排除一个或更多个其它特征、整件、步骤、组件或其组合的存在或附加。It should be emphasized that the term "comprising/comprising" when used herein refers to the presence of features, elements, steps or components, but does not exclude the presence or addition of one or more other features, elements, steps, components or combinations thereof .

这些实施例的许多特征和优点根据该详细描述是清楚的,因此所附权利要求旨在覆盖这些实施例的落入其真实精神和范围内的所有这些特征和优点。此外,由于本领域的技术人员容易想到很多修改和改变,因此不是要将本发明的实施例限于所例示和描述的精确结构和操作,而是可以涵盖落入其范围内的所有合适修改和等同物。The many features and advantages of these embodiments are apparent from this detailed description, and the appended claims are therefore intended to cover all such features and advantages of these embodiments as fall within their true spirit and scope. Furthermore, since many modifications and changes will readily occur to those skilled in the art, the embodiments of the present invention are not intended to be limited to the precise construction and operation illustrated and described, but are to cover all suitable modifications and equivalents falling within the scope thereof thing.

本发明未详细说明部分为本领域技术人员公知技术。The parts of the present invention that are not described in detail are well known to those skilled in the art.

Claims (9)

1.一种降低树脂中挥发份含量的方法,其特征在于,所述方法包括以下步骤:1. a method for reducing volatile matter content in resin, is characterized in that, described method comprises the following steps: 步骤1、设置多辊组件,所述多辊组件至少包括两个压辊,且任意相邻压辊之间具有间距;Step 1. Set up a multi-roller assembly, the multi-roller assembly includes at least two pressing rollers, and there is a gap between any adjacent pressing rollers; 步骤2、将树脂置于多辊组件的任意一组相邻压辊之间,并控制多辊组件的多个压辊进行滚动,其中,任意压辊的温度低于树脂固化温度,树脂在压辊上形成连续的树脂膜;Step 2. The resin is placed between any group of adjacent pressing rollers of the multi-roll assembly, and the plurality of pressing rollers of the multi-roll assembly are controlled to roll, wherein the temperature of any pressing roller is lower than the curing temperature of the resin, and the resin is pressed A continuous resin film is formed on the roller; 步骤3、按照设定时间测量所述相邻压辊之间的树脂中挥发份含量,在所述挥发份含量达到使用要求之前,根据所述挥发份含量调整所述相邻压辊之间的间距,其中,所述挥发份含量与所述间距大小呈负相关,所述树脂挥发份含量在30~40%时,所述相邻压辊的间距为0.1~0.5mm;所述树脂挥发份含量在20~30%时,所述相邻压辊的间距为0.5~2.5mm;所述树脂挥发份含量在5~20%时,所述相邻压辊的间距为2.5~5.0mm。Step 3. Measure the volatile content in the resin between the adjacent pressing rollers according to the set time, and adjust the volatile content between the adjacent pressing rollers according to the volatile content before the volatile content reaches the usage requirements. spacing, wherein the volatile matter content is negatively correlated with the size of the spacing, and when the resin volatile matter content is 30-40%, the spacing between adjacent pressing rollers is 0.1-0.5 mm; the resin volatile matter content is 0.1-0.5 mm; When the content is 20-30%, the distance between the adjacent pressing rollers is 0.5-2.5 mm; when the resin volatile content is 5-20%, the distance between the adjacent pressing rollers is 2.5-5.0 mm. 2.根据权利要求1所述的一种降低树脂中挥发份含量的方法,其特征在于,所述步骤1还包括设置通风设备,所述通风设备用于对所述树脂进行通风。2 . The method for reducing volatile content in resin according to claim 1 , wherein the step 1 further comprises setting a ventilation device, and the ventilation device is used to ventilate the resin. 3 . 3.根据权利要求1所述的一种降低树脂中挥发份含量的方法,其特征在于,,任意所述压辊的温度均为30℃+ΔT,其中,ΔT≤20。3 . The method for reducing volatile content in resin according to claim 1 , wherein, the temperature of any of the pressing rollers is 30° C.+ΔT, wherein ΔT≤20. 4 . 4.根据权利要求1所述的一种降低树脂中挥发份含量的方法,其特征在于,所述多辊组件包括两个压辊。4 . The method for reducing the volatile content in resin according to claim 1 , wherein the multi-roller assembly comprises two pressing rollers. 5 . 5.根据权利要求1所述的一种降低树脂中挥发份含量的方法,其特征在于,所述多辊组件包括三个压辊。5 . The method for reducing volatile content in resin according to claim 1 , wherein the multi-roller assembly comprises three pressing rollers. 6 . 6.根据权利要求5所述的一种降低树脂中挥发份含量的方法,其特征在于,所述包括三个压辊的多辊组件为三压辊研磨机。6 . The method for reducing volatile content in resin according to claim 5 , wherein the multi-roll assembly comprising three pressing rollers is a three-rolling mill. 7 . 7.根据权利要求1所述的一种降低树脂中挥发份含量的方法,其特征在于,所述设定时间为10-30min。7 . The method for reducing volatile content in resin according to claim 1 , wherein the set time is 10-30 min. 8 . 8.根据权利要求1所述的一种降低树脂中挥发份含量的方法,其特征在于,所述树脂为酚醛树脂。8 . The method for reducing volatile content in resin according to claim 1 , wherein the resin is a phenolic resin. 9 . 9.根据权利要求1所述的一种降低树脂中挥发份含量的方法,其特征在于,所述步骤3中,所述树脂中挥发份含量的测量方法为:9. a kind of method that reduces volatile matter content in resin according to claim 1, is characterized in that, in described step 3, the measuring method of volatile matter content in described resin is: 取出一定量树脂,平摊在测量纸上,测定质量为m1;Take out a certain amount of resin, spread it on the measuring paper, and measure the mass as m1; 将树脂及称量纸放入烘箱中,按照设定温度,加热一定时间后,测定其质量为m2;Put the resin and weighing paper into the oven, and after heating for a certain period of time according to the set temperature, measure the mass as m2; 所述树脂中挥发份的含量为((m1-m2)/m1)%。The content of volatile matter in the resin is ((m1-m2)/m1)%.
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