CN101831041B - Preparation method of high-performance phenolic resin - Google Patents
Preparation method of high-performance phenolic resin Download PDFInfo
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- CN101831041B CN101831041B CN2010101382965A CN201010138296A CN101831041B CN 101831041 B CN101831041 B CN 101831041B CN 2010101382965 A CN2010101382965 A CN 2010101382965A CN 201010138296 A CN201010138296 A CN 201010138296A CN 101831041 B CN101831041 B CN 101831041B
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Abstract
The invention relates to a preparation method of high-performance phenolic resin. The method comprises the following steps of: putting 100 parts of phenol and 70-80 parts of formaldehyde to an acidic reaction environment; and respectively carrying out two dewatering polycondensations to prepare high-performance phenolic resin. The phenolic resin has the advantages of suitable viscosity, even molecular weight distribution, low volatile content and stable product quality.
Description
Technical field
The present invention relates to a kind of preparation method of high-performance pnenolic aldehyde resin.
Background technology
Resol has good acidproof, alkaline-resisting, heat-resisting and electrical insulating property, is widely used in fields such as telecommunication, electrical equipment, instrument, daily necessities and light building material.But traditional resol synthesis mode adopts the primary dewatering method to be prepared, and the resol molecular weight that reaction generates is inhomogeneous, and viscosity is not of uniform size, and volatile content is bigger, and impurity is more.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high-performance pnenolic aldehyde resin, the high-performance pnenolic aldehyde resin of preparing has not only that viscosity is big, the characteristics of good toughness, and foreign matter content is low, constant product quality.
Technical program of the present invention lies in: a kind of preparation method of high-performance pnenolic aldehyde resin is characterized in that: carry out according to the following steps:
(1) with 100 parts of phenol, it is 2 ~ 3 that an acidic catalyst makes reaction environment PH, in 70 ~ 80 parts of adding reactors of formaldehyde, heated and stirred 5 ~ 15 minutes, temperature rises to 50 ~ 100 ℃, comes to life in the reactor, and beginning feeds 0.05 ~ 0.2MPa steam in chuck, make to keep in the reactor carrying out widely different stream polycondensation under the ebullient situation, the reaction times is 50 ~ 180 minutes;
(2) progressively vapour pressure is brought up to 0.8MPa from 0.2MPa, simultaneously the vacuum tightness in the conditioned reaction still is from-0.01MPa to-0.08MPa, this process need be carried out 1 hour, with this understanding reactant is carried out for the first time vacuum hydro-extraction to the water content of reactant and reduce to 3 ~ 5%, after this step reaction finished, temperature of charge rose to 125 ~ 130 ℃;
(3) make vapour pressure remain on 0.6MPa, continue to be warming up to 155 ~ 160 ℃ simultaneously, continue heating 60 ~ 120 minutes;
(4) keep temperature-resistant, pressure is reduced to condition of normal pressure, slowly vacuum tightness is reduced to-0.07MPa from-0.01MPa, continue 60-120 minute, reactant is carried out the vacuum hydro-extraction second time, be transparent watery from the beginning until reactor visor phegma, dehydration finishes, the beginning blowing can obtain a kind of high-performance pnenolic aldehyde resin.
Described an acidic catalyst is an oxalic acid.
The invention has the advantages that: use the high-performance pnenolic aldehyde resin of preparation method of the present invention preparation to have not only that viscosity is big, the characteristics of good toughness, and foreign matter content is low, constant product quality, the preparation process technical process is simple, is convenient to operation, is convenient to control.
Embodiment
Further specify the present invention below in conjunction with embodiment:
1, with 100 parts of phenol, 80 parts in formaldehyde, by order of addition(of ingredients) phenol, oxalic acid, formaldehyde drops in the reactor, heats while stirring, and this moment, reacting kettle inner pressure was controlled at about 0.5 ~ 0.8MPa, about about 5 ~ 15 minutes, kettle temperature can rise to 50 ~ 100 ℃, came to life in the pot.Can feed the 0.05-0.2MPa steam heating this moment to chuck, makes reactant keep carrying out widely different stream polycondensation under the ebullient situation, and the reaction times carried out 50-180 minute.
2, vacuum hydro-extraction for the first time
Vacuum tightness slowly increases in carry out in reaction preceding 15 minutes, and vacuum values is from-0.01 to-0.03Mpa, and the final vacuum value reached-0.08Mpa in one hour.Also increase gradually at this process vapor pressure, rise to 0.8Mpa from 0.2Mpa, this moment, kettle temperature dropped to about 65-85 ℃ from about 120 ℃, and large quantity of moisture is deviate from, and this process will be carried out 2.5 hours approximately.Along with constantly deviating from of moisture, kettle temperature will progressively go up, and when material temperature when reaching 125 to 130 ℃, 97% of moisture has been steamed, and the material thickness that becomes stirs difficulty, and dehydration for the first time leaves it at that.
3, heat temperature raising
After the first time, drying and dehydrating finished, material raised up and is brought into condenser during for fear of the removal vacuum, should strengthen quantity of steam, makes vapour pressure remain on 0.6Mpa, made the material temperature rise to 155 ~ 160 ℃ fast.This process will be carried out 60 ~ 120 minutes.This moment, the viscosity of material descended, for condition has been created in the vacuum hydro-extraction second time owing to the rising of temperature.
4, vacuum hydro-extraction for the second time
When normal pressure dehydration material temperature reaches 155 ~ 160 ℃, just can begin dehydration for the second time, vacuum tightness slowly increases, vacuum values is from-0.01 to-0.05Mpa, when vacuum values reach-during 0.07Mpa, the material temperature will reach 165 ℃, observing response still visor phegma is transparent watery from the beginning, dehydration for the second time finishes, and this process will be carried out 60-120 minute.
The relevant after testing index of above-mentioned gained resin is viscosity 33s, 96 ℃ of softening temperatures, free phenol 2.9%, moisture content 1.01%.
In the process of the high-performance pnenolic aldehyde resin that the present invention relates to, to molecular resin amount distribution influence maximum is dehydration under the adjustment of mol ratio and high temperature, the condition of high vacuum degree condition.The change of these 2 processing condition, to molecular-weight average size, the molecular weight distribution of resol, even the structure of molecular chain all can exert an influence.The dehydration operation of high temperature, condition of high vacuum degree greatly reduces water content, free phenol and the low-molecular(weight)polymer content of resin.According to calculating, the moisture of resin reduces 1%; Free phenol is reduced to below 3%.
The above only is preferred embodiment of the present invention, and all equalizations of being done according to the present patent application claim change and modify, and all should belong to covering scope of the present invention.
Claims (1)
1. the preparation method of a high-performance pnenolic aldehyde resin is characterized in that: carry out according to the following steps:
(1) with 100 parts of phenol, it is 2 ~ 3 that an acidic catalyst makes reaction environment pH, in 70 ~ 80 parts of adding reactors of formaldehyde, heated and stirred 5 ~ 15 minutes, temperature rises to 50 ~ 100 ℃, comes to life in the reactor, and beginning feeds 0.05 ~ 0.2MPa steam in chuck, make to keep the polycondensation that refluxes under the ebullient situation in the reactor, the reaction times is 50 ~ 180 minutes;
(2) progressively vapour pressure is brought up to 0.8MPa from 0.2MPa, simultaneously the vacuum tightness in the conditioned reaction still is from-0.01MPa to-0.08MPa, this process need be carried out 1 hour, with this understanding reactant is carried out for the first time vacuum hydro-extraction to the water content of reactant and reduce to 3 ~ 5%, after this step reaction finished, temperature of charge rose to 125 ~ 130 ℃;
(3) make vapour pressure remain on 0.6MPa, continue to be warming up to 155 ~ 160 ℃ simultaneously, continue heating 60 ~ 120 minutes;
(4) keep temperature-resistant, pressure is reduced to condition of normal pressure, slowly vacuum tightness is reduced to-0.07MPa from-0.01MPa, continue 60-120 minute, reactant is carried out the vacuum hydro-extraction second time, be transparent watery from the beginning until reactor visor phegma, dehydration finishes, the beginning blowing promptly obtains a kind of high-performance pnenolic aldehyde resin;
Described an acidic catalyst is an oxalic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101382965A CN101831041B (en) | 2010-04-02 | 2010-04-02 | Preparation method of high-performance phenolic resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101382965A CN101831041B (en) | 2010-04-02 | 2010-04-02 | Preparation method of high-performance phenolic resin |
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| Publication Number | Publication Date |
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| CN101831041A CN101831041A (en) | 2010-09-15 |
| CN101831041B true CN101831041B (en) | 2011-09-07 |
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| CN2010101382965A Expired - Fee Related CN101831041B (en) | 2010-04-02 | 2010-04-02 | Preparation method of high-performance phenolic resin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102558473B (en) * | 2011-12-28 | 2016-08-24 | 北京彤程创展科技有限公司 | A kind of cashew nut oil modified alkyd resin and preparation method thereof |
| CN105153383B (en) * | 2015-09-17 | 2017-09-01 | 浙江杭摩合成材料有限公司 | A kind of preparation method of high-quality phenolic resin |
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| US6239248B1 (en) * | 1998-09-22 | 2001-05-29 | Borden Chemical, Inc. | Phenol-novolacs with improved optical properties |
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Granted publication date: 20110907 Termination date: 20210402 |