CN105367728A - Rosin modified phenol-formaldehyde resin and preparation method therefor - Google Patents
Rosin modified phenol-formaldehyde resin and preparation method therefor Download PDFInfo
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- CN105367728A CN105367728A CN201510850808.3A CN201510850808A CN105367728A CN 105367728 A CN105367728 A CN 105367728A CN 201510850808 A CN201510850808 A CN 201510850808A CN 105367728 A CN105367728 A CN 105367728A
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Abstract
The invention discloses rosin modified phenol-formaldehyde resin. The rosin modified phenol-formaldehyde resin is prepared from the ingredients in percentage by mass: 25-40% of alkylphenol, 5-15% of paraformaldehyde, 0.1-0.5% of alkaline organic catalyst, 45-60% of rosin, 0.1-5% of adjuvants, 3-9% of polyol, 0.1-0.3% of esterification catalyst and 0.1-0.2% of antioxidant. The invention also discloses a preparation method for preparing the resin. According to the rosin modified phenol-formaldehyde resin and the preparation method therefor, the rosin modified phenol-formaldehyde resin product with high solubility, high structure, light color and low cost can be prepared; compared with the two-step method, the preparation method for the rosin modified phenol-formaldehyde resin has the advantages that a resin preparation process is simpler and easier to control, the emission of wastes is less, and the production is safer; and a restricted material, i.e., nonylphenol is not used, so that the production cost is lower.
Description
Technical field
The present invention relates to ink material technical field, particularly relate to a kind of rosin modified phenolic resin.
Background technology
" resin " word origin and secretory product of some trees.Along with the development people of science and technology to synthesize the rosin products of various uses with chemical raw material, thus " resin " one word again neither be original simple meaning, but become the general designation of the material of a family macromolecule amount or macromolecule.
Each attribute of printing-ink, as various resistances such as viscosity, gloss, drying, firmness, rub resistance, water resisting property, major part is played a decisive role by resin.In recent years, along with the high speed of offset printing, in the resin of printing-ink, common demands has various high speed printing adaptive, particularly fly the generation of ink, become the problem that need are studied deeply, in order to suppress the generation flying ink when printing, having started requirement and using high viscosity, low-viscosity ink.For rosin modified phenolic resin, also requirement is the resin of high molecular, high viscosity, high resolution.Mostly be now to adopt two-step approach or single stage method to adopt nonyl phenol, 4-dodecylphenol obtains the rosin modified phenolic resin of high molecular, high viscosity, high resolution, lower cost.But two-step approach and single stage method cut both ways; traditional two-step approach uses liquid formaldehyde because reacting; a large amount of basic catalyst adjusted to ph is needed in reaction; want a large amount of acid to neutralize after reaction terminates and can produce a large amount of waste water; and often can add some benzene kind solvents; make production process more dangerous, and have a large amount of waste water containing phenol and aldehyde to produce, water treatment load is larger.Although new two-step approach have employed disposable technique, use solid formaldehyde in reaction, or can add a certain amount of water is aborning used for improving reaction effect, the wastewater problem of this new two-step approach is not still solved.Traditional single-step resin technics comparing is simple, and phenol and aldehyde react in molten rosin, but because of molten rosin system viscosity higher, dissolve uneven and produce multiple side reaction.And single stage method reaction be phenol formaldehyde condensation, formaldehyde generally can be excessive, excessive formaldehyde can with rosin generation side reaction, there is the disadvantages such as production quality control is poor, the molecular weight of resin is lower, solvability is poor, molecular weight distribution is wide.So need badly a kind ofly can prepare high resolution, high structure, light color, low waste generate, the appearance of the method for the rosin modified phenolic resin of low cost.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of rosin modified phenolic resin, has the feature of high resolution, high structure, low cost.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is:
Thering is provided a kind of rosin modified phenolic resin, is be prepared from by the composition of following massfraction: alkylphenol 25 ~ 40%, paraformaldehyde 5 ~ 15%, basic organic catalyst 0.1 ~ 0.5%, rosin 45 ~ 60%, auxiliary agent 0.1 ~ 5%, polyvalent alcohol 3 ~ 9%, esterifying catalyst 0.1 ~ 0.3% and oxidation inhibitor 0.1 ~ 0.2%.
In a preferred embodiment of the present invention, described rosin originates from Fujian, the place of production, Guangxi, the one-level Pinus massoniana Lamb of In Guangdong Province or the pinus khasys in Yunnan, the place of production.
In a preferred embodiment of the present invention, described alkylphenol is to special tert.-butyl phenol, dihydroxyphenyl propane, mixture to one or more in tert-octylphenol, 4-dodecylphenol.
In a preferred embodiment of the present invention, described auxiliary agent comprises the mixture of one or more in toxilic acid, fumaric acid, dimeracid, dicyclopentadiene, Yatall MA, stearic acid or tung oil.
In a preferred embodiment of the present invention, described polyvalent alcohol is the mixture of one or more in glycerine, Glycerol dimer, monopentaerythritol, dipentaerythritol, TriMethylolPropane(TMP), trimethylolethane or glycol ether etc.
In a preferred embodiment of the present invention, described esterifying catalyst is tosic acid or the vitriol oil.
In a preferred embodiment of the present invention, described oxidation inhibitor is triphenyl phosphite, diisooctyl phenyl phosphite or Wytox 312.
The present invention also provides a kind of preparation method preparing above-mentioned rosin modified phenolic resin, there is the technical indicator basically identical with two step resin, more simply be easy to the production technique controlled, fewer waste discharge, safety, do not use restricted material nonyl phenol, comprise the steps: that alkylphenol being dropped into reactor protection is warming up to 110 DEG C of meltings, open and stir, paraformaldehyde and basic organic catalyst is added after being cooled to 90 DEG C after the complete melting of described alkylphenol, after be warming up to 110 ~ 115 DEG C of pressurization condensation pressure releases after 4 hours, rosin is added again in reactor, heat up while adding described rosin, in 1.5 ~ 2 hours, described rosin is all added and be warming up to 170 DEG C insulation half an hour after add auxiliary agent, 30 minutes are incubated again under the condition of 170 DEG C, polyvalent alcohol is added after rear 1.5 ~ 2 hours temperature to 220 DEG C of slowly heating up, 250 ~ 270 DEG C are warming up to after being incubated 1 hour again under the condition of 220 DEG C, add esterifying catalyst and oxidation inhibitor, esterification is to the acid number of material, viscosity, it is qualified that normal heptane detects, finally vacuumize 30 minutes, remove small molecules material wherein, obtain finished colophonium modified phenolic resins.
The invention has the beneficial effects as follows: a kind of rosin modified phenolic resin of the present invention and preparation method thereof, the processing method of traditional single-step resin is improved, formulation optimization, innovation, the rosin modified phenolic resin product of a kind of high resolution, high structure, the production of low waste, light low cost can be prepared, the technique that its production method produces resin compared with two-step approach is more simply easy to control, waste discharge is less, production is safer, and do not use restricted material nonyl phenol, there is lower production cost.
Embodiment
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
Embodiment 1:
A kind of rosin modified phenolic resin is be prepared from by the composition of following massfraction: alkylphenol 35%, paraformaldehyde 10.1%, basic organic catalyst 0.2%, rosin 49%, auxiliary agent 1.0%, polyvalent alcohol 4.5%, esterifying catalyst 0.1% and oxidation inhibitor 0.1%.
Described rosin originates from Fujian, the place of production, Guangxi, the one-level Pinus massoniana Lamb of In Guangdong Province or the pinus khasys in Yunnan, the place of production.
Described alkylphenol is to special tert.-butyl phenol, dihydroxyphenyl propane, mixture to one or more in tert-octylphenol, 4-dodecylphenol.
Described auxiliary agent comprises the mixture of one or more in toxilic acid, fumaric acid, dimeracid, dicyclopentadiene, Yatall MA, stearic acid or tung oil.
Described polyvalent alcohol is the mixture of one or more in glycerine, Glycerol dimer, monopentaerythritol, dipentaerythritol, TriMethylolPropane(TMP), trimethylolethane or glycol ether etc.
Described esterifying catalyst is tosic acid or the vitriol oil.
Described oxidation inhibitor is triphenyl phosphite, diisooctyl phenyl phosphite or Wytox 312.
Embodiment 2:
A kind of rosin modified phenolic resin is be prepared from by the composition of following massfraction: to tert-octylphenol 31%, paraformaldehyde 9.4%, basic organic catalyst 0.2%, rosin 54.2%, toxilic acid 0.2%, glycerine 4.8%, tosic acid 0.1% and triphenyl phosphite 0.1%.
All the other moietys are with embodiment 1.
Embodiment 3:
A kind of rosin modified phenolic resin is be prepared from by the composition of following massfraction: to tert-octylphenol 30%, paraformaldehyde 9.6%, basic organic catalyst 0.15%, rosin 52%, tung oil 3%, glycerine 3.5%, TriMethylolPropane(TMP) 1.5%, tosic acid 0.15% and oxidation inhibitor 0.1%.
All the other moietys are with embodiment 1.
A kind of preparation method of the rosin modified phenolic resin prepared in above-mentioned any embodiment, phenol and aldehyde improve reaction completeness in high-temperature pressurizing condensation in reactor under the effect of organic basic catalyzer, control formaldehyde consumption, reduce formaldehyde emissions, and in phenolic aldehyde slurry, rosin is dripped in comparatively high temps situation, rear high temperature carries out esterification; Utilize esterifying catalyst enhance esterification speed and improve molecular weight, specifically comprising the steps:
Alkylphenol is dropped into reactor protection and be warming up to 110 DEG C of meltings, open and stir, paraformaldehyde and basic organic catalyst is added after being cooled to 90 DEG C after the complete melting of described alkylphenol, after be warming up to 110 ~ 115 DEG C of pressurization condensation pressure releases after 4 hours, rosin is added again in reactor, heat up while adding described rosin, in 1.5 ~ 2 hours, described rosin is all added and be warming up to 170 DEG C insulation half an hour after add auxiliary agent, 30 minutes are incubated again under the condition of 170 DEG C, polyvalent alcohol is added after rear 1.5 ~ 2 hours temperature to 220 DEG C of slowly heating up, 250 ~ 270 DEG C are warming up to after being incubated 1 hour again under the condition of 220 DEG C, add esterifying catalyst and oxidation inhibitor, esterification is to the acid number of material, viscosity, it is qualified that normal heptane detects, finally vacuumize 30 minutes, remove small molecules material wherein, obtain finished colophonium modified phenolic resins.
Following table is the technical indicator deck watch between the rosin modified phenolic resin for preparing of rosin modified phenolic resin that in embodiment 1 ~ 3, any embodiment prepares and conventional two-step.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (8)
1. a rosin modified phenolic resin, it is characterized in that, be prepared from by the composition of following massfraction: alkylphenol 25 ~ 40%, paraformaldehyde 5 ~ 15%, basic organic catalyst 0.1 ~ 0.5%, rosin 45 ~ 60%, auxiliary agent 0.1 ~ 5%, polyvalent alcohol 3 ~ 9%, esterifying catalyst 0.1 ~ 0.3% and oxidation inhibitor 0.1 ~ 0.2%.
2. rosin modified phenolic resin according to claim 1, is characterized in that, described rosin originates from Fujian, the place of production, Guangxi, the one-level Pinus massoniana Lamb of In Guangdong Province or the pinus khasys in Yunnan, the place of production.
3. rosin modified phenolic resin according to claim 1, is characterized in that, described alkylphenol is to special tert.-butyl phenol, dihydroxyphenyl propane, mixture to one or more in tert-octylphenol, 4-dodecylphenol.
4. rosin modified phenolic resin according to claim 1, is characterized in that, described auxiliary agent comprises the mixture of one or more in toxilic acid, fumaric acid, dimeracid, dicyclopentadiene, Yatall MA, stearic acid or tung oil.
5. rosin modified phenolic resin according to claim 1, is characterized in that, described polyvalent alcohol is the mixture of one or more in glycerine, Glycerol dimer, monopentaerythritol, dipentaerythritol, TriMethylolPropane(TMP), trimethylolethane or glycol ether etc.
6. rosin modified phenolic resin according to claim 1, is characterized in that, described esterifying catalyst is tosic acid or the vitriol oil.
7. rosin modified phenolic resin according to claim 1, is characterized in that, described oxidation inhibitor is triphenyl phosphite, diisooctyl phenyl phosphite or Wytox 312.
8. prepare the preparation method of the described rosin modified phenolic resin of one of claim 1 ~ 7 for one kind, it is characterized in that, comprise the steps: that alkylphenol being dropped into reactor protection is warming up to 110 DEG C of meltings, open and stir, paraformaldehyde and basic organic catalyst is added after being cooled to 90 DEG C after the complete melting of described alkylphenol, after be warming up to 110 ~ 115 DEG C of pressurization condensation pressure releases after 4 hours, rosin is added again in reactor, heat up while adding described rosin, in 1.5 ~ 2 hours, described rosin is all added and be warming up to 170 DEG C insulation half an hour after add auxiliary agent, 30 minutes are incubated again under the condition of 170 DEG C, polyvalent alcohol is added after rear 1.5 ~ 2 hours temperature to 220 DEG C of slowly heating up, 250 ~ 270 DEG C are warming up to after being incubated 1 hour again under the condition of 220 DEG C, add esterifying catalyst and oxidation inhibitor, esterification is to the acid number of material, viscosity, it is qualified that normal heptane detects, finally vacuumize 30 minutes, remove small molecules material wherein, obtain finished colophonium modified phenolic resins.
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| CN201510850808.3A CN105367728A (en) | 2015-11-30 | 2015-11-30 | Rosin modified phenol-formaldehyde resin and preparation method therefor |
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Cited By (5)
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|---|---|---|---|---|
| CN106065056A (en) * | 2016-06-07 | 2016-11-02 | 桂林市产品质量检验所 | A kind of offset printing rosin modified phenolic resin preparation of sections method |
| CN106279588A (en) * | 2016-08-29 | 2017-01-04 | 广西梧州通轩林产化学有限公司 | The preparation method of coating rosin modified phenolic resin |
| CN107778975A (en) * | 2016-08-30 | 2018-03-09 | 天津天女化工集团股份有限公司 | A kind of ink printing connection material formula and preparation method thereof |
| CN112480733A (en) * | 2020-12-10 | 2021-03-12 | 天津天女化工集团股份有限公司 | High-grade environment-friendly printing ink |
| CN113402686A (en) * | 2021-07-27 | 2021-09-17 | 封开海蓝化工有限公司 | Modified rosin phenolic resin and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106065056A (en) * | 2016-06-07 | 2016-11-02 | 桂林市产品质量检验所 | A kind of offset printing rosin modified phenolic resin preparation of sections method |
| CN106279588A (en) * | 2016-08-29 | 2017-01-04 | 广西梧州通轩林产化学有限公司 | The preparation method of coating rosin modified phenolic resin |
| CN107778975A (en) * | 2016-08-30 | 2018-03-09 | 天津天女化工集团股份有限公司 | A kind of ink printing connection material formula and preparation method thereof |
| CN112480733A (en) * | 2020-12-10 | 2021-03-12 | 天津天女化工集团股份有限公司 | High-grade environment-friendly printing ink |
| CN113402686A (en) * | 2021-07-27 | 2021-09-17 | 封开海蓝化工有限公司 | Modified rosin phenolic resin and preparation method thereof |
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