CN104194642B - The preparation method of rich horse Colophonium - Google Patents
The preparation method of rich horse Colophonium Download PDFInfo
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- CN104194642B CN104194642B CN201410423780.0A CN201410423780A CN104194642B CN 104194642 B CN104194642 B CN 104194642B CN 201410423780 A CN201410423780 A CN 201410423780A CN 104194642 B CN104194642 B CN 104194642B
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Abstract
The invention discloses the preparation method of a kind of rich horse Colophonium, relate to Colophonium deep process technology field, preparation method comprises the following steps: be sequentially added into fumaric acid and toluene in reactor, it is warming up to 60 DEG C～70 DEG C, stir, be subsequently adding molten rosin and catalyst, stir, it is warming up to 120 DEG C～130 DEG C, it is passed through microwave, reacts 30 minutes～40 minutes, washing, distillation, obtains rich horse Colophonium.The present invention is using zinc oxide and cobalt acetate as catalyst, and introduces microwave in course of reaction so that reaction is fully carried out, thus improves feed stock conversion, and the final productivity improving product, obtained product softening point is higher, and color and luster is shallower.
Description
Technical field
The present invention relates to Colophonium deep process technology field, the preparation method of a kind of rich horse Colophonium.
Background technology
Rich horse Colophonium is a kind of important fine chemical product synthesized by esterification by Colophonium and fumaric acid, rich horse Colophonium can be applicable to the senior welding compound of electronic product, and the derivant product of its synthesis more can be widely used in the fields such as ink, coating, printing and dyeing, adhesive.But in the richest horse Colophonium preparation process, catalyst is inefficient, and reaction can not fully be carried out, and ultimately results in feed stock conversion low.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of rich horse Colophonium, this preparation method can solve the problem that feed stock conversion is low.
In order to solve the problems referred to above, the technical solution used in the present invention is: the preparation method of a kind of rich horse Colophonium, comprises the following steps: be sequentially added into fumaric acid and toluene in reactor, it is warming up to 60 DEG C～70 DEG C, stir, be subsequently adding molten rosin and catalyst, stir, it is warming up to 120 DEG C～130 DEG C, it is passed through microwave, reacts 30 minutes～40 minutes, washing, distillation, obtains rich horse Colophonium.
Further, described catalyst is the mixture of zinc oxide and cobalt acetate.
Further, described fumaric acid, toluene, the mass ratio of molten rosin and catalyst is 1:1～2:0.8～1.2:0.05:0.2.
Further, the power of described microwave is 500 watts～700 watts.
Owing to have employed technique scheme, the present invention compared with prior art has the advantages that
1, the present invention is using zinc oxide and cobalt acetate as catalyst, and to introduce power in course of reaction be 500 watts～the microwave of 700 watts so that reaction is fully carried out, and improves feed stock conversion, the final productivity improving product.
2, present invention process is simple, and low cost, prepared product softening point is higher, and color and luster is shallower.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
In reactor, it is sequentially added into 1 kilogram of fumaric acid and 1.5 kilograms of toluene, is warming up to 60 DEG C, stirs, be subsequently adding 0.8 kilogram of molten rosin and 50 grams of catalyst, stir, be warming up to 130 DEG C, be passed through the microwave that power is 500 watts, react 30 minutes, washing, distillation, obtain rich horse Colophonium.
Catalyst described in the present embodiment be mass ratio be zinc oxide and the mixture of cobalt acetate of 1:1.
In the present embodiment, the conversion ratio of fumaric acid is 94%, and the softening point of obtained rich horse Colophonium is 87.3 DEG C.
Embodiment 2
In reactor, it is sequentially added into 10 kilograms of fumaric acid and 20 kilograms of toluene, is warming up to 70 DEG C, stirs, be subsequently adding 12 kilograms of molten rosin and 1 kg catalyst, stir, be warming up to 120 DEG C, be passed through the microwave that power is 600 watts, react 35 minutes, washing, distillation, obtain rich horse Colophonium.
Catalyst described in the present embodiment be mass ratio be zinc oxide and the mixture of cobalt acetate of 2:1.
In the present embodiment, the conversion ratio of fumaric acid is 95.1%, and the softening point of obtained rich horse Colophonium is 86.7 DEG C.
Embodiment 3
In reactor, it is sequentially added into 50 kilograms of fumaric acid and 50 kilograms of toluene, is warming up to 65 DEG C, stirs, be subsequently adding 50 kilograms of molten rosin and 10 kg catalyst, stir, be warming up to 125 DEG C, be passed through the microwave that power is 700 watts, react 40 minutes, washing, distillation, obtain rich horse Colophonium.
Catalyst described in the present embodiment be mass ratio be zinc oxide and the mixture of cobalt acetate of 1:2.
In the present embodiment, the conversion ratio of fumaric acid is 95.2%, and the softening point of obtained rich horse Colophonium is 86.5 DEG C.
Claims (2)
1. the preparation method of a rich horse Colophonium, it is characterized in that comprising the following steps: in reactor, be sequentially added into fumaric acid and toluene, be warming up to 60 DEG C～70 DEG C, stir, it is subsequently adding molten rosin and catalyst, stir, be warming up to 120 DEG C～130 DEG C, be passed through microwave, react 30 minutes～40 minutes, washing, distillation, obtain rich horse Colophonium；Wherein, described catalyst is the mixture of zinc oxide and cobalt acetate；The power of microwave is 500 watts～700 watts.
The preparation method of rich horse Colophonium the most according to claim 1, it is characterised in that: the mass ratio of described fumaric acid, toluene, molten rosin and catalyst is 1:1～2:0.8～1.2:0.05～0.2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410423780.0A CN104194642B (en) | 2014-08-26 | 2014-08-26 | The preparation method of rich horse Colophonium |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410423780.0A CN104194642B (en) | 2014-08-26 | 2014-08-26 | The preparation method of rich horse Colophonium |
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| CN104194642A CN104194642A (en) | 2014-12-10 |
| CN104194642B true CN104194642B (en) | 2016-08-24 |
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| CN201410423780.0A Active CN104194642B (en) | 2014-08-26 | 2014-08-26 | The preparation method of rich horse Colophonium |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372605A (en) * | 2008-10-22 | 2009-02-25 | 昆明理工大学 | Method for preparing rosin glyceride by microwave irradiation |
| CN103965787A (en) * | 2014-05-08 | 2014-08-06 | 江西殷莱特化工有限公司 | Method for rapidly producing rosin resin |
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2014
- 2014-08-26 CN CN201410423780.0A patent/CN104194642B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372605A (en) * | 2008-10-22 | 2009-02-25 | 昆明理工大学 | Method for preparing rosin glyceride by microwave irradiation |
| CN103965787A (en) * | 2014-05-08 | 2014-08-06 | 江西殷莱特化工有限公司 | Method for rapidly producing rosin resin |
Non-Patent Citations (2)
| Title |
|---|
| "富马酸改性松香树脂的合成";陈学恒;《现代化工》;20040731;第24卷(第增刊（1）期);第116-119页 * |
| "改性富马松香的研究与应用";耿世铭等;《精细化工》;19891231;第6卷(第2期);第48-50页 * |
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| CN104194642A (en) | 2014-12-10 |
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