CN111320734B - Method for reducing volatile content in resin - Google Patents
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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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- 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
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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Abstract
The invention provides a method for reducing the content of volatile matters in resin, which comprises the following steps: step 1, arranging a multi-roller assembly, wherein the multi-roller assembly at least comprises two press rollers; step 2, placing the resin between any group of adjacent compression rollers of the multi-roller assembly, and controlling the multiple compression rollers of the multi-roller assembly to roll, wherein the temperature of any compression roller is lower than the curing temperature of the resin; and 3, measuring the volatile matter content in the resin between the adjacent press rollers according to set time, and adjusting the spacing between the adjacent press rollers according to the volatile matter content before the volatile matter content meets the use requirement, wherein the volatile matter content is in negative correlation with the spacing. The method provided by the invention is simple and feasible, the volatile content removal efficiency is high, the obtained resin does not influence the subsequent use, and the technical problem existing in the existing resin volatile content removal method can be solved.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a method for reducing the content of volatile matters in resin.
Background
The resin (usually referred to as phenolic resin) may contain excessive reacted phenolic substances, and a certain amount of solvent is required to be mixed in the production process for discharging convenience, which is the main component of volatile matters in the phenolic resin. However, with the development of composite material technology, the wet prepreg has poor quality stability and is difficult to meet the requirement of environmental protection, and the process for preparing the prepreg by the wet method is gradually replaced by the process for preparing the prepreg by a melting method. However, most of the resins in the market still contain a large amount of solvent, and the problem to be solved firstly is to reduce the content of volatile components in the resin by adopting a hot-melt method to prepare the resin prepreg. At present, the method for reducing the volatile content of the resin is to pour the resin into an iron pan and put the resin into a vacuum oven for vacuumizing to remove the solvent, and the method has the following problems:
1) the solvent removal efficiency is low. The solvent in the resin can be removed quickly in the early stage by adopting a vacuumizing mode, but the viscosity of the system is increased along with the reduction of the solvent content of the surface layer resin, and the skinning of the surface layer resin prevents the solvent at the bottom layer from volatilizing outwards, so that the solvent removal efficiency is reduced sharply;
2) affecting the subsequent use of the resin. In order to accelerate the volatilization of the solvent, the temperature of the oven is set to about 60 ℃ during the vacuum pumping, the requirement of preparing the resin prepreg by a hot melting method can be met only when the removal time is generally 16-24h, but the curing degree of the resin is slowly improved by long-time high-temperature treatment, and the curing performance of the resin is influenced.
Disclosure of Invention
The following presents a simplified summary of the invention in order to provide a basic understanding of some aspects of the invention. It should be understood that this summary is not an exhaustive overview of the invention. It is not intended to determine the key or critical elements of the present invention, nor is it intended to limit the scope of the present 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.
The invention aims to overcome the defects in the prior art, provides a method for reducing the volatile content in resin, is simple and feasible, has high volatile content removal efficiency, does not influence subsequent use, and solves the technical problem existing in the prior method for removing the volatile content in resin.
The technical solution of the invention is as follows: a method for reducing the volatile content of resin is provided, which comprises the following steps:
step 1, arranging a multi-roller assembly, wherein the multi-roller assembly at least comprises two press rollers;
step 2, placing the resin between any group of adjacent compression rollers of the multi-roller assembly, and controlling the multiple compression rollers of the multi-roller assembly to roll, wherein the temperature of any compression roller is lower than the curing temperature of the resin;
and 3, measuring the volatile matter content in the resin between the adjacent press rollers according to set time, and adjusting the spacing between the adjacent press rollers according to the volatile matter content before the volatile matter content meets the use requirement, wherein the volatile matter content is in negative correlation with the spacing.
Further, the step 1 further comprises providing a ventilation device for ventilating the resin.
Further, the temperature of any press roll is 30 ℃ + Δ T, wherein Δ T is less than or equal to 20.
Further, the multi-roll assembly includes two press rolls.
Further, the multi-roll assembly includes three press rolls.
Further, the multi-roll assembly comprising three press rolls is a three press roll grinder.
Further, the set time is 10-30 min.
Further, the resin is a phenolic resin.
Further, when the content of the resin volatile matter is 30-40%, the distance between the adjacent compression rollers is 0.1-0.5 mm; when the content of the resin volatile matter is 20-30%, the distance between the adjacent compression rollers is 0.5-2.5 mm; when the content of the volatile matter in the resin is 5-20%, the distance between the adjacent press rolls is 2.5-5.0 mm.
Further, in the step 3, the method for measuring the content of the volatile components in the resin comprises the following steps:
taking out a certain amount of resin, spreading the resin on a measuring paper, and measuring the mass to be m 1;
putting the resin and the weighing paper into an oven, heating for a certain time according to a set temperature, and measuring the mass of the resin and the weighing paper to be m 2;
the content of volatile components in the resin is ((m1-m2)/m 1)%.
By applying the technical scheme, the method capable of reducing the volatile content of the resin at low temperature is provided, the multi-roller assembly comprising at least two pressing rollers is adopted, the pressing rollers rotating at high speed are utilized to enable the resin to be continuously extruded between the pressing rollers and continuously form a continuous resin film on the pressing rollers, the removal efficiency is ensured by continuously adjusting the distance between the adjacent pressing rollers according to the volatile content, the resin obtains the same probability of contacting air by the mode, and the volatile content of the resin can be synchronously reduced and the efficiency is high. Further, since the nip roll temperature setting is low and the processing time is short, there is little influence on the subsequent curing property of the resin. In conclusion, the preparation method disclosed by the invention is simple to operate, has small influence on subsequent use of the resin, is economic and environment-friendly, has high volatile matter removal efficiency (the content of the volatile matter is reduced to be lower than 10%), and is wide in application field.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is a schematic diagram of a multi-roll assembly employing two rolls for removing resin volatiles content in accordance with an embodiment of the present invention;
FIG. 2 is a schematic diagram of resin volatiles removal from a multi-roll assembly using three rolls in accordance with an embodiment of the present invention.
Detailed Description
The following provides a detailed description of specific embodiments of the present invention. In the following description, for purposes of explanation and not limitation, specific details are set forth in order to provide a thorough understanding of the present invention. However, it will be apparent to one skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the device structures and/or processing steps that are closely related to the scheme according to the present invention are shown in the drawings, and other details that are not so relevant to the present invention are omitted.
As the background art relates to, the existing method for removing the volatile content in the resin is to pour the resin into an iron pan and put the iron pan into a vacuum oven for vacuumizing to remove the volatile content, and firstly, the solvent removal efficiency is low; secondly, the subsequent use of the resin is influenced by overhigh temperature. Based on the background, the embodiment of the invention provides a method for reducing the volatile content of resin, the method provided by the invention is simple and feasible, the volatile content removal efficiency is high, the obtained resin does not influence the subsequent use, and the technical problem existing in the existing method for removing the volatile content of resin is solved. The method for reducing the volatile matter content of the resin provided by the embodiment of the invention comprises the following steps:
step 1, arranging a multi-roller assembly, wherein the multi-roller assembly at least comprises two press rollers;
step 2, placing the resin between any group of adjacent compression rollers of the multi-roller assembly, and controlling the multiple compression rollers of the multi-roller assembly to roll, wherein the temperature of any compression roller is lower than the curing temperature of the resin;
and 3, measuring the volatile matter content in the resin between the adjacent press rollers according to set time, and adjusting the spacing between the adjacent press rollers according to the volatile matter content before the volatile matter content meets the use requirement, wherein the volatile matter content is in negative correlation with the spacing.
In the embodiment of the present invention, the resin may be a phenolic resin.
In the embodiment of the invention, the plurality of press rolls included in the multi-roll assembly are horizontally arranged, and each press roll is in the same horizontal plane, namely the section of the highest point of each press roll is in the same horizontal plane.
In the embodiment of the present invention, as shown in fig. 1-2, the rolling directions of any adjacent rollers are opposite rolling directions, for example, one roller rolls counterclockwise and the roller adjacent to the roller rolls clockwise. In addition, the specific means for controlling the press roll may be known in the art and will not be described in detail herein.
In embodiments of the invention, the resin disposed between adjacent rolls should not exceed the highest point of any roll.
In the embodiment of the present invention, the adjacent press rolls of the multi-roll assembly are two press rolls moving opposite to each other, as shown in the figure, a first roll and a second roll, or a second roll and a third roll, and further, unless otherwise stated, the adjacent press rolls of the embodiment of the present invention refer to a group of adjacent press rolls on which the resin is placed as described in step 2.
In the embodiment of the invention, the initial spacing between all the adjacent press rolls can be determined according to the initial content of the volatile resin, for example, in the case of phenolic resin, the initial content of the volatile resin is 30-40%, and the initial spacing is set to be 0.1-0.5 mm.
The method for reducing the volatile content of the resin at low temperature adopts a multi-roller assembly comprising at least two press rollers, the resin is continuously extruded between the press rollers by the press rollers rotating at high speed to continuously form a continuous resin film on the press rollers (it should be noted that in the method, the resin is not completely adhered to the press rollers, and the resin is partially extruded and separated from the press rollers when entering a small space, so as to form a dynamic resin film), so that the resin obtains the same probability of contacting air, the volatile content of the resin can be synchronously reduced, the efficiency is high, and the space between adjacent press rollers is continuously adjusted according to the volatile content, on the premise of ensuring that the resin is retained in a gap between the first roller and the second roller, the thickness of the resin film on the surface of the compression roller is increased as much as possible, the film forming time of the resin on the roller is prolonged, and the removal efficiency is ensured. In addition, since the temperature setting of the press roll is low, there is little influence on the subsequent curing property of the resin.
As an embodiment of the present invention, in order to further improve the removal efficiency of volatile components in the resin, the step 1 further includes providing a ventilation device for ventilating the resin. Through this kind of design, through increasing resin and air area of contact to guarantee that the resin obtains the probability of the same contact air, under ventilation and the heating circumstances, guaranteed the efficiency of getting rid of volatile.
As an embodiment of the invention, in order to ensure the removal efficiency of volatile matters and not influence the subsequent use of resin, the temperature of any press roll is 30 ℃ plus delta T, wherein delta T is less than or equal to 20. Therefore, the method provided by the embodiment of the invention can remove the volatile matters in the resin at low temperature, and ensures the subsequent use effect of the resin.
As an example, the nip temperature may be set to 30 to 50 c for phenolic resins.
As an embodiment of the present invention, the multi-roll assembly includes no more than three press rolls. One, then. And secondly, the resin is basically extruded and formed on the adjacent press rolls, and the resin content on the subsequent press rolls is not high (only the distance between the adjacent press rolls needs to be adjusted in a corresponding method). Combining two factors, it is preferable to set the number of the press rolls to not more than three.
As a specific example, the multi-roll assembly includes two press rolls, as shown in fig. 1.
As a specific example, the multi-roll assembly includes three press rolls, as shown in fig. 2.
More specifically, the multi-roll assembly including three rolls may be a three-roll mill, which is a conventional apparatus, as shown in fig. 2, and the method of the embodiment of the present invention based on the three-roll mill is exemplified as follows:
1: starting the three-roll grinder, controlling the gap between a front roll (a first roll, the same below) and a second roll at an initial interval, enabling a scraper to leave the roll surface of a rear roll (a third roll), slowly pouring a certain amount of phenolic resin between the front roll and the second roll of the three-roll grinder, and enabling the phenolic resin to cover the gap and be flush with the highest point of the front roll;
2: testing the volatile matter content of the resin once every set time, and adjusting the distance between rollers according to the volatile matter content; wherein, the phenolic resin continuously rolls on a three-roller grinding machine, the roller temperature is controlled at 30-50 ℃, the three-roller grinding machine is utilized to grind and generate heat to volatilize the phenolic resin, and meanwhile, ventilation equipment is started to accelerate the air flow speed;
3: and after the volatile matter of the phenolic resin meets the requirement, the scraper is attached to the back roller, and the phenolic resin is scraped off from the three-roller grinding machine and flows into a collecting device.
As an embodiment of the invention, the set time can be 10-30min, and can also be 20-30 min.
As an embodiment of the present invention, in order to improve the removal efficiency of the volatile components in the resin, the volatile component content in the resin and the pitch of the adjacent press rolls may be set to have the following relationship: when the content of the resin volatile matter is 30-40%, the distance between the adjacent compression rollers is 0.1-0.5 mm; when the content of the resin volatile matter is 20-30%, the distance between the adjacent compression rollers is 0.5-2.5 mm; when the content of the volatile matter in the resin is 5-20%, the distance between the adjacent press rolls is 2.5-5.0 mm. By the configuration mode, under the specific relation between the volatile matter content and the distance between the adjacent press rolls, the removal efficiency of the volatile matter content can be ensured to be optimal.
As an embodiment of the present invention, in order to accurately obtain the content of the volatile components in the resin in step 3, the method for measuring the content of the volatile components in the resin may be:
taking out a certain amount of resin, spreading the resin on a measuring paper, and measuring the mass to be m 1;
putting the resin and the weighing paper into an oven, heating for a certain time according to a set temperature, and measuring the mass of the resin and the weighing paper to be m 2;
the content of volatile components in the resin is ((m1-m2)/m 1)%.
In summary, the method of the embodiment of the invention utilizes the press rolls rotating at high speed to continuously press the resin between the press rolls, the roll rolling of the press rolls forms a continuous resin film on the surface, the roll distance is adjusted according to the volatile content of the resin, and the volatile content in the phenolic resin is reduced from 40% to below 10% at a lower temperature under the combined action of the roll temperature at the bottom of the resin film and the air flow above the roll temperature. The method does not need a special solvent removing device, is suitable for coarse solvent removal, and has the advantages of low temperature, high efficiency and little influence on the subsequent curing performance of the phenolic resin. The method can be widely applied to the fields of national defense industry, military, aerospace, building and the like.
The present invention is described in further detail below with reference to specific examples, which are not to be construed as limiting the scope of the invention as claimed.
The following examples take phenolic resin as an example, and the multi-roll assembly comprises three press rolls, and particularly a three-roll grinder can be adopted.
Example 1
Step 1: starting a three-roll grinding machine, controlling the gap between a front roll and a second roll to be 0.1mm, enabling a scraper to leave the roll surface of a rear roll, slowly pouring a certain amount of phenolic resin between the front roll and the second roll of the three-roll grinding machine, wherein the phenolic resin covers the gap and is flush with the highest point of the front roll;
step 2: the resin volatile content was tested every 30min and the roll spacing was adjusted according to the volatile content. The method for testing the volatile content in the phenolic resin comprises the steps of taking out 10-20 g of phenolic resin, spreading the phenolic resin on measuring paper, and measuring the mass m 1. The resin and the weighing paper were put in an oven at 100 ℃ for 10 minutes and then taken out, and the mass was measured as m 2. The content of volatile components in the resin is (m1-m2)/m 1%. When the volatile content of the resin is 30-40%, the roller spacing is 0.1 mm; when the volatile content of the resin is 20-30%, the roller spacing is 0.5 mm; when the volatile matter content of the resin is 10-20%, the distance between the rollers is 2.5mm, wherein the phenolic resin continuously rolls on a three-roller grinding machine, the roller temperature is controlled at 30 ℃, the three-roller grinding machine is used for grinding to generate heat to volatilize the phenolic resin, and meanwhile, a ventilation device is started to accelerate the air flow speed;
and step 3: and after the volatile matter of the phenolic resin meets the requirement, the scraper is attached to the back roller, and the phenolic resin is scraped off from the three-roller grinding machine and flows into a collecting device.
The gel time, the treatment time for reducing the volatile content of the phenolic resin from 40% to 10% and the production efficiency of the phenolic resin are compared in the embodiment shown in Table 1.
Example 2
Step 1: starting the three-roller grinding machine, controlling the gap between the front roller and the second roller to be 0.1mm, enabling the scraper to be away from the roller surface of the rear roller, slowly pouring a certain amount of phenolic resin between the front roller and the second roller of the three-roller grinding machine, wherein the amount of phenolic resin covers the gap and is flush with the highest point of the front roller;
step 2: the resin volatile content was tested every 30min and the roll spacing was adjusted according to the volatile content. The method for testing the volatile content in the phenolic resin comprises the steps of taking out 10-20 g of phenolic resin, spreading the phenolic resin on measuring paper, and measuring the mass m 1. The resin and the weighing paper were put in an oven, the temperature was set at 100 ℃, and after 10 minutes, they were taken out, and their mass was measured as m 2. The content of volatile components in the resin is (m1-m2)/m 1%. When the volatile content of the resin is 30-40%, the roller spacing is 0.1 mm; when the volatile content of the resin is 20-30%, the roller spacing is 0.5 mm; when the volatile matter content of the resin is 10-20%, the distance between the rollers is 2.5mm, wherein the phenolic resin continuously rolls on a three-roller grinding machine, the roller temperature is controlled at 40 ℃, the three-roller grinding machine is used for grinding to generate heat to volatilize the phenolic resin, and meanwhile, a ventilation device is started to accelerate the air flow speed;
and step 3: and after the volatile matter of the phenolic resin meets the requirement, the scraper is attached to the back roller, and the phenolic resin is scraped off from the three-roller grinding machine and flows into a collecting device.
The gel time, the treatment time for reducing the volatile content of the phenolic resin from 40% to 10% and the production efficiency of the phenolic resin are compared in the embodiment shown in Table 1.
Example 3
Step 1: starting the three-roller grinding machine, controlling the gap between the front roller and the second roller to be 0.1mm, enabling the scraper to be away from the roller surface of the rear roller, slowly pouring a certain amount of phenolic resin between the front roller and the second roller of the three-roller grinding machine, wherein the amount of phenolic resin covers the gap and is flush with the highest point of the front roller;
step 2: the volatile content of the resin was measured every 30min and the roll spacing was adjusted according to the volatile content. The method for testing the volatile content in the phenolic resin comprises the steps of taking out 10-20 g of phenolic resin, spreading the phenolic resin on measuring paper, and measuring the mass m 1. The resin and the weighing paper were put in an oven at 100 ℃ for 10 minutes and then taken out, and the mass was measured as m 2. The content of volatile components in the resin is (m1-m2)/m 1%. When the volatile content of the resin is 30-40%, the roller spacing is 0.1 mm; when the volatile content of the resin is 20-30%, the roller spacing is 0.5 mm; when the volatile matter content of the resin is 10-20%, the distance between the rollers is 2.5mm, wherein the phenolic resin continuously rolls on a three-roller grinding machine, the roller temperature is controlled at 50 ℃, the three-roller grinding machine is used for grinding to generate heat to volatilize the phenolic resin, and meanwhile, a ventilation device is started to accelerate the air flow speed;
and 3, step 3: and after the volatile matter of the phenolic resin meets the requirement, the scraper is attached to the back roller, and the phenolic resin is scraped off from the three-roller grinding machine and flows into a collecting device.
The gel time, the processing time for reducing the volatile content of the phenolic resin from 40% to 10% and the production efficiency of the phenolic resin are compared in the table 1.
Example 4
Step 1: starting the three-roller grinding machine, controlling the gap between the front roller and the second roller to be 0.5mm, enabling the scraper to be away from the roller surface of the rear roller, slowly pouring a certain amount of phenolic resin between the front roller and the second roller of the three-roller grinding machine, wherein the amount of phenolic resin covers the gap and is flush with the highest point of the front roller;
step 2: the resin volatile content was tested every 30min and the roll spacing was adjusted according to the volatile content. The method for testing the volatile content in the phenolic resin comprises the steps of taking out 10-20 g of phenolic resin, spreading the phenolic resin on measuring paper, and measuring the mass m 1. The resin and the weighing paper were put in an oven at 100 ℃ for 10 minutes and then taken out, and the mass was measured as m 2. The content of volatile components in the resin is (m1-m2)/m 1%. When the volatile content of the resin is 30-40%, the roller spacing is 0.5 mm; when the volatile content of the resin is 20-30%, the roller spacing is 2.5 mm; when the volatile matter content of the resin is 10-20%, the roller spacing is 5.0mm, wherein the phenolic resin continuously rolls on a three-roller grinding machine, the roller temperature is controlled at 50 ℃, the three-roller grinding machine is used for grinding to generate heat to volatilize the phenolic resin, and meanwhile, a ventilation device is started to accelerate the air flow speed;
and step 3: and after the volatile matter of the phenolic resin meets the requirement, the scraper is attached to the back roller, and the phenolic resin is scraped off from the three-roller grinding machine and flows into a collecting device.
The gel time, the processing time for reducing the volatile content of the phenolic resin from 40% to 10% and the production efficiency of the phenolic resin are compared in the table 1.
Comparative example
Putting 2Kg of phenolic resin into a vacuum oven, setting the temperature to 80 ℃, taking out after 6h, and measuring that the volatile content of the phenolic resin is 25 percent, the gelation time at 120 ℃ is 7min, and the production efficiency is 0.5 Kg/h.
Table 1 test results of each example
It can be seen from table 1 that the higher the roll temperature of the three-roll mill, the larger the roll gap, the higher the removal efficiency of the volatile matter of the phenolic resin, and the gel time of the phenolic resin is reduced after the roll temperature is increased, but the use is not affected. The production efficiency is shown in the table by the amount of the phenolic resin which reduces the volatile content to less than 10% per unit time. When the roller diameter and the length of the three-roller grinding machine are fixed, the production efficiency depends on the roller gap and the roller temperature, and the larger the roller gap is, the higher the temperature is, and the higher the production efficiency is.
As can be seen from Table 1 and the comparative examples, the resin of the comparative example has higher volatile content after 6h treatment, the production efficiency is lower than that of the invention, and the resin gel time is obviously shortened, which shows that the curing performance of the resin is influenced by the treatment process and the use of the subsequent resin is influenced.
Features that are described and/or illustrated above with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments and/or in combination with or instead of the features of the other embodiments.
It should be emphasized that the term "comprises/comprising" when used herein, is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, integers, steps, components or groups thereof.
The many features and advantages of these embodiments are apparent from the detailed specification, and thus, it is intended by the appended claims to cover all such features and advantages of these embodiments which fall within the true spirit and scope thereof. Further, since numerous modifications and changes will readily occur to those skilled in the art, it is not desired to limit the embodiments of the invention to the exact construction and operation illustrated and described, and accordingly, all suitable modifications and equivalents may be resorted to, falling within the scope thereof.
The invention has not been described in detail and is not limited thereto.
Claims (9)
1. A method for reducing the volatile content of a resin, comprising the steps of:
step 1, arranging a multi-roller assembly, wherein the multi-roller assembly at least comprises two press rollers, and a space is formed between any two adjacent press rollers;
step 2, placing the resin between any group of adjacent compression rollers of the multi-roller assembly, and controlling the plurality of compression rollers of the multi-roller assembly to roll, wherein the temperature of any compression roller is lower than the curing temperature of the resin, and the resin forms a continuous resin film on the compression rollers;
step 3, measuring the volatile content in the resin between the adjacent compression rollers according to set time, and adjusting the spacing between the adjacent compression rollers according to the volatile content before the volatile content meets the use requirement, wherein the volatile content is in negative correlation with the spacing, and when the volatile content of the resin is 30-40%, the spacing between the adjacent compression rollers is 0.1-0.5 mm; when the content of the resin volatile matter is 20-30%, the distance between the adjacent compression rollers is 0.5-2.5 mm; when the volatile content of the resin is 5-20%, the distance between the adjacent press rolls is 2.5-5.0 mm.
2. The method for reducing the volatile content of the resin according to claim 1, wherein the step 1 further comprises providing a ventilation device for ventilating the resin.
3. The method of claim 1, wherein the temperature of any of the rolls is 30 ℃ + Δ T, where Δ T is 20 or less.
4. The method of claim 1, wherein the multi-roll assembly comprises two press rolls.
5. The method of claim 1, wherein the multi-roll assembly comprises three press rolls.
6. The method of claim 5, wherein the multi-roll assembly comprising three rolls is a three roll mill.
7. The method for reducing the volatile content in the resin according to claim 1, wherein the set time is 10-30 min.
8. The method of claim 1, wherein the resin is a phenolic resin.
9. The method for reducing the volatile content in the resin according to claim 1, wherein in the step 3, the volatile content in the resin is measured by:
taking out a certain amount of resin, spreading the resin on a measuring paper, and measuring the mass to be m 1;
putting the resin and the weighing paper into an oven, heating for a certain time according to a set temperature, and measuring the mass of the resin and the weighing paper to be m 2;
the content of volatile components in the resin is ((m1-m2)/m 1)%.
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| CN102108185B (en) * | 2010-12-29 | 2012-07-04 | 黑龙江省科学院石油化学研究院 | Epoxy matrix resin and prepreg and preparation method thereof and device for preparation thereof |
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