CN105001388A - Preparation method for vegetable oil modified rosin phenolic resin - Google Patents
Preparation method for vegetable oil modified rosin phenolic resin Download PDFInfo
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- CN105001388A CN105001388A CN201510548038.7A CN201510548038A CN105001388A CN 105001388 A CN105001388 A CN 105001388A CN 201510548038 A CN201510548038 A CN 201510548038A CN 105001388 A CN105001388 A CN 105001388A
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Abstract
The invention provides a preparation method for vegetable oil modified rosin phenolic resin. The preparation method comprises the following steps of firstly, feeding rosin into a reaction kettle, raising the temperature to be 180DEG C, adding vegetable oil, continuously raising the temperature to be 210 to 215DEG C and keeping the temperature for 1 to 1.5 hours, and carrying out addition reaction; secondly, feeding pentaerythritol and magnesium oxide into the reaction kettle, reducing the temperature to be 160 to 170DEG C, feeding dodecylphenol and p-tert-butylphenol according to the mole ratio of 1:1.01 to 1.03, then continuously reducing the temperature to be 120 to 130DEG C, feeding paraformaldehyde according to the mole ratio of phenol to aldehyde being 1:2.0 to 2.1, and keeping the temperature for 2 to 2.5 hours; thirdly, raising the temperature in the reaction kettle to be 260 to 270DEG C, keeping the temperature, carrying out esterification reaction until an acid value is smaller than 25mgKOH/g, and carrying out reduced pressure distillation to obtain a low-boiling-point substance, namely the vegetable oil modified rosin phenolic resin. The resin prepared by the preparation method provided by the invention has the advantages of high viscosity, good solubility, high molecular weight, uniformity in distribution and suitability for offset lithography of ink.
Description
Technical field
The present invention relates to a kind of preparation method of modified rosin resin, be specifically related to a kind of preparation method of plant oil modified rosin phenolic resin.
Background technology
Offset litho printing ink resin mainly rosin modified phenolic resin, its complete processing under the effect of basic catalyst, carries out condensation reaction with alkylphenol and formaldehyde, then addition reaction is carried out with sylvic acid, carry out esterification by the carboxyl on polyvalent alcohol and rosin afterwards, and finally generate macromolecule product.Due to the characteristic of the typography of traditional offset litho printing ink, binder needs lower acid number, high viscosity, structural/snappiness and high mineral oil accommodation degree (usually representing with normal heptane accommodation degree).For a long time, rosin modified phenolic resin mainly adopts single alkylphenol modification, as dodecyl phenol, nonylphenol, to tert-octylphenol, p-tert-butylphenol etc., but the Gum Rosin of single alkylphenol modification, is difficult to realize that viscosity is high and solvability good simultaneously.This be due to alkyl carbon chain longer time, the solvability of resin is good, but viscosity is low, when alkyl carbon chain is shorter, resin poorly soluble, but viscosity is high.
Summary of the invention
The technical problem to be solved in the present invention is to provide the good and preparation method of the plant oil modified rosin phenolic resin that viscosity is high of a kind of solvability.
Technical scheme provided by the invention is the preparation method of plant oil modified rosin phenolic resin, comprises the following steps:
1) rosin is dropped in reactor, be warming up to 180 DEG C, add vegetables oil, continue to be warming up to 210 ~ 215 DEG C and be incubated 1 ~ 1.5h and carry out addition reaction;
2) in reactor, tetramethylolmethane and magnesium oxide is added, be cooled to 160 ~ 170 DEG C, in molar ratio for the ratio of 1:1.01 ~ 1.03 adds dodecyl phenol and p-tert-butylphenol, then continue to be cooled to 120 ~ 130 DEG C, the ratio being 1:2.0 ~ 2.1 in phenolic aldehyde mol ratio again adds paraformaldehyde, and is incubated 2 ~ 2.5h at such a temperature;
3) reactor temperature is risen to 260 ~ 270 DEG C and insulation is carried out esterification and is less than 25mgKOH/g to acid number, underpressure distillation goes out low-boiling-point substance, obtains plant oil modified rosin phenolic resin.
Step 1) in, the weight ratio of rosin and vegetables oil is 100:5 ~ 30.Described vegetables oil is soya-bean oil, oleum lini or Viscotrol C.
Step 2) in, the mol ratio of rosin and tetramethylolmethane is 1:1.1 ~ 1.3.
Compared with prior art, not only softening temperature is high for the plant oil modified rosin phenolic resin that the present invention obtains, and acid number is low, and viscosity is high, and solvability is good, and molecular weight is between 135730 ~ 196913, and molecular weight is large, and is evenly distributed, and is applicable to offset lithographic ink.
Embodiment
The present invention is further elaborated for following specific embodiment, but not as a limitation of the invention.
Embodiment 1
1) drop in reactor by rosin, be warming up to 180 DEG C, add soya-bean oil, rosin and soya-bean oil weight ratio are 100:5, continue to be warming up to 210 DEG C and are incubated 1h and carry out addition reaction;
2) in reactor, tetramethylolmethane and magnesium oxide is added, the mol ratio of rosin and tetramethylolmethane is 1:1.1, be cooled to 160 DEG C, in molar ratio for the ratio of 1:1.01 adds dodecyl phenol and p-tert-butylphenol, then continue to be cooled to 120 DEG C, the ratio being 1:2.0 in phenolic aldehyde mol ratio again adds paraformaldehyde, and is incubated 2h at such a temperature;
3) reactor temperature is risen to 260 DEG C and insulation is carried out esterification and is less than 25mgKOH/g to acid number, underpressure distillation goes out low-boiling-point substance, obtains plant oil modified rosin phenolic resin.
Embodiment 2
1) drop in reactor by rosin, be warming up to 180 DEG C, add oleum lini, the weight ratio of rosin and oleum lini is 100:30, continues to be warming up to 215 DEG C and is incubated 1.5h and carry out addition reaction;
2) in reactor, tetramethylolmethane and magnesium oxide is added, the mol ratio of rosin and tetramethylolmethane is 1:1.3, be cooled to 170 DEG C, in molar ratio for the ratio of 1:1.03 adds dodecyl phenol and p-tert-butylphenol, then continue to be cooled to 130 DEG C, the ratio being 1:2.1 in phenolic aldehyde mol ratio again adds paraformaldehyde, and is incubated 2.5h at such a temperature;
3) reactor temperature is risen to 270 DEG C and insulation is carried out esterification and is less than 25mgKOH/g to acid number, underpressure distillation goes out low-boiling-point substance, obtains plant oil modified rosin phenolic resin.
Embodiment 3
1) drop in reactor by rosin, be warming up to 180 DEG C, add Viscotrol C, the weight ratio of rosin and Viscotrol C is 100:20, continues to be warming up to 213 DEG C and is incubated 1.3h and carry out addition reaction;
2) in reactor, tetramethylolmethane and magnesium oxide is added, the mol ratio of rosin and tetramethylolmethane is 1:1.2, be cooled to 165 DEG C, in molar ratio for the ratio of 1:1.02 adds dodecyl phenol and p-tert-butylphenol, then continue to be cooled to 125 DEG C, the ratio being 1:2.05 in phenolic aldehyde mol ratio again adds paraformaldehyde, and is incubated 2.2h at such a temperature;
3) reactor temperature is risen to 265 DEG C and insulation is carried out esterification and is less than 25mgKOH/g to acid number, underpressure distillation goes out low-boiling-point substance, obtains plant oil modified rosin phenolic resin.
The resin of embodiment 1 ~ 3 is carried out following comparison with existing resin:
Claims (4)
1. the preparation method of plant oil modified rosin phenolic resin, is characterized in that: comprise the following steps:
1) rosin is dropped in reactor, be warming up to 180 DEG C, add vegetables oil, continue to be warming up to 210 ~ 215 DEG C and be incubated 1 ~ 1.5h and carry out addition reaction;
2) in reactor, tetramethylolmethane and magnesium oxide is added, be cooled to 160 ~ 170 DEG C, in molar ratio for the ratio of 1:1.01 ~ 1.03 adds dodecyl phenol and p-tert-butylphenol, then continue to be cooled to 120 ~ 130 DEG C, the ratio being 1:2.0 ~ 2.1 in phenolic aldehyde mol ratio again adds paraformaldehyde, and is incubated 2 ~ 2.5h at such a temperature;
3) reactor temperature is risen to 260 ~ 270 DEG C and insulation is carried out esterification and is less than 25mgKOH/g to acid number, underpressure distillation goes out low-boiling-point substance, obtains plant oil modified rosin phenolic resin.
2. the preparation method of plant oil modified rosin phenolic resin according to claim 1, is characterized in that: step 1) in, the weight ratio of rosin and vegetables oil is 100:5 ~ 30.
3. the preparation method of plant oil modified rosin phenolic resin according to claim 2, is characterized in that: described vegetables oil is soya-bean oil, oleum lini or Viscotrol C.
4. the preparation method of plant oil modified rosin phenolic resin according to claim 1, is characterized in that: step 2) in, the mol ratio of rosin and tetramethylolmethane is 1:1.1 ~ 1.3.
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Cited By (4)
| 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 |
| CN107473679A (en) * | 2017-08-31 | 2017-12-15 | 苏州仲勉装饰有限公司 | A kind of preparation method of magnesia combination rosin modified phenolic resin compound insulating material |
| CN112708257A (en) * | 2020-12-31 | 2021-04-27 | 宁波能之光新材料科技股份有限公司 | High-elasticity wear-resistant outdoor wood-plastic surface layer material and preparation method thereof |
| CN113667076A (en) * | 2021-02-23 | 2021-11-19 | 广西藤县通轩立信化学有限公司 | Preparation method of phosphorus-modified rosin phenolic resin catalyzed by acid and then base |
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| CN101054430A (en) * | 2007-05-23 | 2007-10-17 | 福建师范大学 | Method of preparing rosin modified phenolic resins with high viscosity and high dissolvability |
| CN101717482A (en) * | 2009-11-30 | 2010-06-02 | 天津东洋油墨有限公司 | Preparation method of high viscosity and high solubility resin used for offset heat set ink |
| CN102911330A (en) * | 2012-10-16 | 2013-02-06 | 山西省应用化学研究所 | Vegetable oil modified rosin phenolic resin and preparation method thereof |
| CN103059240A (en) * | 2012-12-04 | 2013-04-24 | 张健 | Preparation method of maleated rosin pentaerythritol modified phenolic resin |
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2015
- 2015-08-31 CN CN201510548038.7A patent/CN105001388B/en active Active
Patent Citations (4)
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| CN101054430A (en) * | 2007-05-23 | 2007-10-17 | 福建师范大学 | Method of preparing rosin modified phenolic resins with high viscosity and high dissolvability |
| CN101717482A (en) * | 2009-11-30 | 2010-06-02 | 天津东洋油墨有限公司 | Preparation method of high viscosity and high solubility resin used for offset heat set ink |
| CN102911330A (en) * | 2012-10-16 | 2013-02-06 | 山西省应用化学研究所 | Vegetable oil modified rosin phenolic resin and preparation method thereof |
| CN103059240A (en) * | 2012-12-04 | 2013-04-24 | 张健 | Preparation method of maleated rosin pentaerythritol modified phenolic resin |
Cited By (6)
| 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 |
| CN107473679A (en) * | 2017-08-31 | 2017-12-15 | 苏州仲勉装饰有限公司 | A kind of preparation method of magnesia combination rosin modified phenolic resin compound insulating material |
| CN107473679B (en) * | 2017-08-31 | 2020-04-03 | 苏州仲勉装饰有限公司 | Preparation method of magnesium oxide and rosin combined modified phenolic resin composite thermal insulation material |
| CN112708257A (en) * | 2020-12-31 | 2021-04-27 | 宁波能之光新材料科技股份有限公司 | High-elasticity wear-resistant outdoor wood-plastic surface layer material and preparation method thereof |
| CN112708257B (en) * | 2020-12-31 | 2022-06-17 | 宁波能之光新材料科技股份有限公司 | High-elasticity wear-resistant outdoor wood-plastic surface layer material and preparation method thereof |
| CN113667076A (en) * | 2021-02-23 | 2021-11-19 | 广西藤县通轩立信化学有限公司 | Preparation method of phosphorus-modified rosin phenolic resin catalyzed by acid and then base |
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| CN105001388B (en) | 2017-03-01 |
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