CN103820032A - Preparation method of pentaerythrite colophony europium resin - Google Patents
Preparation method of pentaerythrite colophony europium resin Download PDFInfo
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- CN103820032A CN103820032A CN201410078259.8A CN201410078259A CN103820032A CN 103820032 A CN103820032 A CN 103820032A CN 201410078259 A CN201410078259 A CN 201410078259A CN 103820032 A CN103820032 A CN 103820032A
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- colophony
- pentaerythrite
- rosin
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- Adhesives Or Adhesive Processes (AREA)
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Abstract
The invention discloses a preparation method of pentaerythrite colophony europium resin , which comprises the followings: by weight, heating 100 parts of colophony to 150-160 DEG C to melt, adding 20-22 parts of europia and 10-15 parts of bisphenol A, rising the temperature to 180-200 DEG C, agitating for 0.3-0.5 hour, cooling to 90-100 DEG C, adding 12-30 parts of formaldehyde and 1-3 parts of accelerant hexamethylene tetramine, agitating 2-2.5 hours at a constant temperature of 90-100 DEG C, adding 10-15 parts of pentaerythrite, agitating and reacting fro 2-2.5 hours, rising the temperature to 270-280 DEG C, and vacuumizing for 1 hour, and obtaining the product. The pentaerythrite colophony europium resin preparation method has the advantages that the design is scientific and reasonable, the reaction speed is high and mild, the control is easy, the product has light color, the softening point can reach above 185 DEG C, the quality is good, and the production cost is lowered.
Description
Technical field
The invention belongs to a kind of rosin deep processing method.
Background technology
Rosin is the renewable resources of China's abundant, and annual production reaches more than 60 ten thousand tons, ranks first in the world.It has unique chemical structure and mulitiple chiral centers by a series of resin acid compositions, and the carboxyl in structure and phenanthrene ring frame can carry out a series of chemical modification, is a kind of natural chiral source material.Rosin can obtain a series of deep processed products through chemical modification, is widely used in the every field in daily life, plays very important effect in the national economic development.The value ratio raw material rosin of these deep processed products is mentioned 2-10 doubly, even decades of times, and China mainly earns foreign exchange with outlet gum resin at present.China is the country of gum resin export volume maximum, accounts for 60% left and right of volume of world trade, and many developed countries are from China's imported raw material rosin, and after a series of deep processings, product is exported go back to again China back, and the conservation of resources to China and Economic development are very unfavorable.China is 35% to rosin deep processing and utilization rate, and by contrast, the developed countries such as America and Europe approach 100% to the deep processing and utilization rate of rosin, exist very large gap.Therefore, carry out Abietyl modified research, develop the not only development to country and local economy of deep processing rosin product that meets China market demand, and reasonable development to China's forest resourceies and utilization and at present industrial energy saving lower consumption and be all of great significance.That one has two chemical reactivity centers as the resinous acid of rosin main component---the chemically reactive substance of carboxylic acid and two keys, just can introduce atom or group at quarter by these two chain carriers, thereby give rosin and there is desirable character, reach the object of modification, thereby change the rational performance of rosin, greatly expand the Application Areas of rosin, formed miscellaneous rosin derived product, be widely used in pressure sensitive adhesive, tackiness agent industry.Manufacture multiple film glue, decorating glue, label glue, adhesive tape glue, hot melt adhesive, sanitary towel glue, non-setting adhesive, EVA hot melt adhesive, polyamide hot, seal gum, varnish paint vehicle, bookbinding glue, pipeline glue etc.In recent decades, rosin deep processing aspect, its product category, preparation method are all without large progress; , there is the deficiencies such as sluggish length consuming time in prior art products preparation method.
Through Chinese publication retrieval, find 527 of relevant patents of invention, do not find the scheme identical with present patent application.
Summary of the invention
The object of the invention is to: for the deficiencies in the prior art, propose a kind of rosin pentaerythritol ester europium process for preparing resins.
Rosin pentaerythritol ester europium process for preparing resins of the present invention, it is characterized in that: by weight, 100 parts of rosin, heat 150-160 ℃ of meltings, add 20-22 parts of europium sesquioxides, 10-15 parts of dihydroxyphenyl propanes, heat up 180-200 ℃, stir 0.3-0.5 hour, be cooled to 90-100 ℃, add 12-30 parts, formaldehyde, 1-3 parts of promotor hexamethylenetetramines, 90-100 ℃ of stirrings of constant temperature 2-2.5 hours, add 10-15 parts of tetramethylolmethanes, stirring reaction 2-2.5 hours, is warming up to 270-280 ℃ and vacuumizes 1 hour; Both obtained product.
Product of the present invention has lighter color, and softening temperature high is applied to the industrial sectors such as paint, ink, synthetic resins, tackiness agent, electronics, chemical industry.
The present invention's beneficial effect compared with prior art: design science is reasonable, speed of response is fast and relax, and is easy to control, and product look shallow, softening temperature is above up to 185 ℃, quality is good, the advantages such as production cost reduction.
Embodiment
Embodiment
The raw materials used acquisition of buying of the present invention.
Rosin pentaerythritol ester europium process for preparing resins of the present invention, it is characterized in that: by weight, 100 parts of rosin, heat 150-160 ℃ of meltings, add 20-22 parts of europium sesquioxides, 10-15 parts of dihydroxyphenyl propanes, heat up 180-200 ℃, stir 0.3-0.5 hour, be cooled to 90-100 ℃, add 12-30 parts, formaldehyde, 1-3 parts of promotor hexamethylenetetramines, 90-100 ℃ of stirrings of constant temperature 2-2.5 hours, add 10-15 parts of tetramethylolmethanes, stirring reaction 2-2.5 hours, is warming up to 270-280 ℃ and vacuumizes 1 hour; Both obtained product.
Products obtained therefrom quality index reaches following index:
Claims (1)
1. a rosin pentaerythritol ester europium process for preparing resins, it is characterized in that: by weight, 100 parts of rosin, heat 150-160 ℃ of meltings, add 20-22 parts of europium sesquioxides, 10-15 parts of dihydroxyphenyl propanes, heat up 180-200 ℃, stir 0.3-0.5 hour, be cooled to 90-100 ℃, add 12-30 parts, formaldehyde, 1-3 parts of promotor hexamethylenetetramines, 90-100 ℃ of stirrings of constant temperature 2-2.5 hours, add 10-15 parts of tetramethylolmethanes, stirring reaction 2-2.5 hours, is warming up to 270-280 ℃ and vacuumizes 1 hour; Both obtained product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410078259.8A CN103820032B (en) | 2014-03-05 | 2014-03-05 | Rosin pentaerythritol ester europium process for preparing resins |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410078259.8A CN103820032B (en) | 2014-03-05 | 2014-03-05 | Rosin pentaerythritol ester europium process for preparing resins |
Publications (2)
| Publication Number | Publication Date |
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| CN103820032A true CN103820032A (en) | 2014-05-28 |
| CN103820032B CN103820032B (en) | 2015-09-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410078259.8A Expired - Fee Related CN103820032B (en) | 2014-03-05 | 2014-03-05 | Rosin pentaerythritol ester europium process for preparing resins |
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Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105331146A (en) * | 2015-11-29 | 2016-02-17 | 韦富林 | Aminohexylaminomethyltriethoxy silane assistant agent |
| CN105331124A (en) * | 2015-11-29 | 2016-02-17 | 韦谷林 | Diethyl amino methyl triethoxy silane auxiliary |
| CN105331123A (en) * | 2015-11-07 | 2016-02-17 | 李安平 | Dioctyltin calcium carbonate activating agent |
| CN105330897A (en) * | 2015-11-07 | 2016-02-17 | 陶荣燕 | Sodium acrylate calcium carbonate activating agent |
| CN105348706A (en) * | 2015-11-07 | 2016-02-24 | 陶荣燕 | Polyvinyl acetal resin calcium carbonate activating agent |
| CN105348824A (en) * | 2015-11-07 | 2016-02-24 | 李安平 | Dipropylene glycol monopropyl ether calcium carbonate activating agent |
| CN105348826A (en) * | 2015-11-07 | 2016-02-24 | 陶荣燕 | Fungacetin calcium carbonate activating agent |
| CN105348823A (en) * | 2015-11-07 | 2016-02-24 | 李安平 | Rosin europium resin calcium carbonate activating agent |
| CN105348825A (en) * | 2015-11-07 | 2016-02-24 | 李安平 | Betaine calcium carbonate activating agent |
| CN105368074A (en) * | 2015-11-26 | 2016-03-02 | 陶荣芝 | Bisethylene titanate powder modifier |
| CN105368093A (en) * | 2015-11-26 | 2016-03-02 | 严亚木 | Isopropyl tri(dioctyl acyloxy phosphate) titanate non-metal powder activator |
| CN105367827A (en) * | 2015-11-26 | 2016-03-02 | 廖文成 | Titanium triisostearoylisopropoxide compound powder activator |
| CN105368094A (en) * | 2015-11-26 | 2016-03-02 | 龙启知 | Gamma-chloropropyl trimethoxy siloxane powder modifier |
| CN105368095A (en) * | 2015-11-26 | 2016-03-02 | 杨毅 | Bis(triethoxy sily propyl) disulphide powder modifier |
| CN105367962A (en) * | 2015-11-26 | 2016-03-02 | 李�杰 | Bis-(gamma-triethoxysilylpropyl) tetrasulfide powder modifier |
| CN105367963A (en) * | 2015-11-26 | 2016-03-02 | 何丽萍 | Titanium triisostearoylisopropoxide non-metal powder activator |
| CN105384966A (en) * | 2015-11-07 | 2016-03-09 | 陶荣燕 | Coconut oil-calcium carbonate activating agent |
| CN105419397A (en) * | 2015-11-07 | 2016-03-23 | 陶荣燕 | Calcium carbonate activating agent containing dipropylene glycol monobutyl ether |
| CN105419194A (en) * | 2015-11-26 | 2016-03-23 | 李伟强 | Isopropyl dioleic(acyloxy) titanate non-metallic powder activator |
| CN105419396A (en) * | 2015-11-07 | 2016-03-23 | 李安平 | Carboxylated imidozoline phosphate activator for calcium carbonate |
| CN105440738A (en) * | 2015-11-26 | 2016-03-30 | 严积芳 | Tetraisopropyl di(dioctylphosphate) titanate powder modifier |
| CN105482328A (en) * | 2015-11-26 | 2016-04-13 | 李小群 | Isopropyl trioleyl titanate nonmetal powder activator |
| CN105482329A (en) * | 2015-11-26 | 2016-04-13 | 廖煜明 | Distearoyl isopropoxy aluminate aid |
| CN105504880A (en) * | 2015-11-26 | 2016-04-20 | 廖煜明 | Gamma-chloropropyl triethoxysilane auxiliary agent |
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| CN1458918A (en) * | 2000-07-19 | 2003-11-26 | 实验室发展科学公司 | Method for preparing fatty substance ester and use thereof in pharmaceutics, cosmetics or food industry |
| CN102977299A (en) * | 2012-12-04 | 2013-03-20 | 李先兰 | Preparation method of rosin pentaerythritol phenol formaldehyde resin |
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2014
- 2014-03-05 CN CN201410078259.8A patent/CN103820032B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1458918A (en) * | 2000-07-19 | 2003-11-26 | 实验室发展科学公司 | Method for preparing fatty substance ester and use thereof in pharmaceutics, cosmetics or food industry |
| CN102977299A (en) * | 2012-12-04 | 2013-03-20 | 李先兰 | Preparation method of rosin pentaerythritol phenol formaldehyde resin |
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384966A (en) * | 2015-11-07 | 2016-03-09 | 陶荣燕 | Coconut oil-calcium carbonate activating agent |
| CN105419396A (en) * | 2015-11-07 | 2016-03-23 | 李安平 | Carboxylated imidozoline phosphate activator for calcium carbonate |
| CN105331123A (en) * | 2015-11-07 | 2016-02-17 | 李安平 | Dioctyltin calcium carbonate activating agent |
| CN105330897A (en) * | 2015-11-07 | 2016-02-17 | 陶荣燕 | Sodium acrylate calcium carbonate activating agent |
| CN105348706A (en) * | 2015-11-07 | 2016-02-24 | 陶荣燕 | Polyvinyl acetal resin calcium carbonate activating agent |
| CN105348824A (en) * | 2015-11-07 | 2016-02-24 | 李安平 | Dipropylene glycol monopropyl ether calcium carbonate activating agent |
| CN105348826A (en) * | 2015-11-07 | 2016-02-24 | 陶荣燕 | Fungacetin calcium carbonate activating agent |
| CN105348823A (en) * | 2015-11-07 | 2016-02-24 | 李安平 | Rosin europium resin calcium carbonate activating agent |
| CN105348825A (en) * | 2015-11-07 | 2016-02-24 | 李安平 | Betaine calcium carbonate activating agent |
| CN105419397A (en) * | 2015-11-07 | 2016-03-23 | 陶荣燕 | Calcium carbonate activating agent containing dipropylene glycol monobutyl ether |
| CN105368094A (en) * | 2015-11-26 | 2016-03-02 | 龙启知 | Gamma-chloropropyl trimethoxy siloxane powder modifier |
| CN105368074A (en) * | 2015-11-26 | 2016-03-02 | 陶荣芝 | Bisethylene titanate powder modifier |
| CN105504880A (en) * | 2015-11-26 | 2016-04-20 | 廖煜明 | Gamma-chloropropyl triethoxysilane auxiliary agent |
| CN105368095A (en) * | 2015-11-26 | 2016-03-02 | 杨毅 | Bis(triethoxy sily propyl) disulphide powder modifier |
| CN105367962A (en) * | 2015-11-26 | 2016-03-02 | 李�杰 | Bis-(gamma-triethoxysilylpropyl) tetrasulfide powder modifier |
| CN105367963A (en) * | 2015-11-26 | 2016-03-02 | 何丽萍 | Titanium triisostearoylisopropoxide non-metal powder activator |
| CN105368093A (en) * | 2015-11-26 | 2016-03-02 | 严亚木 | Isopropyl tri(dioctyl acyloxy phosphate) titanate non-metal powder activator |
| CN105367827A (en) * | 2015-11-26 | 2016-03-02 | 廖文成 | Titanium triisostearoylisopropoxide compound powder activator |
| CN105419194A (en) * | 2015-11-26 | 2016-03-23 | 李伟强 | Isopropyl dioleic(acyloxy) titanate non-metallic powder activator |
| CN105482329A (en) * | 2015-11-26 | 2016-04-13 | 廖煜明 | Distearoyl isopropoxy aluminate aid |
| CN105440738A (en) * | 2015-11-26 | 2016-03-30 | 严积芳 | Tetraisopropyl di(dioctylphosphate) titanate powder modifier |
| CN105482328A (en) * | 2015-11-26 | 2016-04-13 | 李小群 | Isopropyl trioleyl titanate nonmetal powder activator |
| CN105331124A (en) * | 2015-11-29 | 2016-02-17 | 韦谷林 | Diethyl amino methyl triethoxy silane auxiliary |
| CN105331146A (en) * | 2015-11-29 | 2016-02-17 | 韦富林 | Aminohexylaminomethyltriethoxy silane assistant agent |
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| CN103820032B (en) | 2015-09-30 |
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Effective date of registration: 20170627 Address after: 526600 fine chemical dangerous chemicals area, County Industrial Park, Deqin County, Zhaoqing, Guangdong Patentee after: DEQING MINGLIANG RESIN CO.,LTD. Address before: Xiangyang Road, eight step zone 542800 the Guangxi Zhuang Autonomous Region Hezhou City No. 1 Patentee before: Zhang Yajing |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
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Granted publication date: 20150930 |