CN104151208A - Preparation method for sulfonated dehydroabietic acid - Google Patents
Preparation method for sulfonated dehydroabietic acid Download PDFInfo
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- CN104151208A CN104151208A CN201410386057.XA CN201410386057A CN104151208A CN 104151208 A CN104151208 A CN 104151208A CN 201410386057 A CN201410386057 A CN 201410386057A CN 104151208 A CN104151208 A CN 104151208A
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- intermediate product
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- dehydroabietic acid
- sulfonated
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Abstract
The invention discloses a preparation method for sulfonated dehydroabietic acid, and belongs to the technical field of rosin deep processing. The preparation method comprises the following steps: placing disproportionate rosin, acid clay and 1-methyl-3-octyl imidazole hydrogen sulfate salt ionic liquid into a reaction still, stirring uniformly and backflowing to obtain an intermediate product I; adding toluene into the intermediate I for extraction to collect an upper-layered material; extracting and drying the upper-layered material to obtain an intermediate product II; then, placing the intermediate product II in freezing concentrated sulfuric acid and stirring under an ice bath condition; next, switching to a boiling water bath condition, adding activated carbon, stirring, filtering, collecting filtrate and performing cooling crystallization; recrystallizing and finally drying to obtain the sulfonated dehydroabietic acid. The purity of the sulfonated dehydroabietic acid prepared by the invention is higher than 94 %.
Description
Technical field
The invention belongs to rosin deep process technology field, relate in particular to a kind of preparation method of sulfonation dehydroabietic acid.
Background technology
Rosin is to take pine resin as raw material, the non-volatile natural resin obtaining by different processing modes.Rosin is important industrial chemicals, is widely used in the industries such as soap, papermaking, paint, rubber.
Rosin has multiple derivative, and sulfonation dehydroabietic acid is one of them, and it is applied thereby have very widely because having the advantages such as stable in properties, resistance of oxidation is strong, specific rotatory power is large.But, because oxidizing reaction easily occurs rosin in deep-processing process, cause the color of the ester gum that makes excessively dark, cannot reach the demand in market.
Yet, preparation method's complicated process of preparation of existing sulfonation dehydroabietic acid, the shortcoming such as product foreign matter content is high, preparation cost height, makes the production of sulfonation dehydroabietic acid and uses to be all subject to certain restrictions.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of sulfonation dehydroabietic acid, the preparation method that this preparation method can solve because of existing sulfonation dehydroabietic acid exists complicated process of preparation, product foreign matter content is high, the shortcomings such as preparation cost height, make the production of sulfonation dehydroabietic acid and use the problem being all subject to certain restrictions.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
It comprises the following steps:
A. under agitation condition, by 50 weight part～65 weight part nilox resins, 35 weight part～40 weight part acid clays and 10 weight part～20 weight part 1-methyl-3-octyl group imidazole bisulfate ionic liquids are put into reactor, be uniformly mixed, then at 95 ℃～105 ℃, reflux 10 hours～12 hours, obtain intermediate product I;
After B.A step, in described intermediate product I, add 2 times～3 times toluene to extract, collect upper strata material;
After C.B step, repeat B step 1 time～2 times, by the upper strata material of finally collecting concentrate, dry, obtain intermediate product II;
After D.C step, the intermediate product II making is put into the freezing vitriol oil in advance, under condition of ice bath, stir 0.5 hour～1 hour;
After E.D step, go to immediately under boiling water bath condition, add 5 weight part～8 weight part gacs, stir 1 hour～3 hours, then filter described gac, collect filtrate crystallisation by cooling, then recrystallization, final drying, obtains.
Owing to adopting technique scheme, the beneficial effect that the present invention obtains is:
The purity of the sulfonation dehydroabietic acid that the present invention makes reaches more than 94%.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, and protection scope of the present invention is not only confined to following examples.
Embodiment 1
The preparation method of this sulfonation dehydroabietic acid comprises the following steps:
A. under agitation condition, by 50kg nilox resin, 35kg acid clay and 10kg1-methyl-3-octyl group imidazole bisulfate ionic liquid are put into reactor, are uniformly mixed, and then at 95 ℃, reflux 12 hours, obtain intermediate product I;
After B.A step, in described intermediate product I, add 2 times of toluene to extract, collect upper strata material;
After C.B step, repeat B step 1 time, the upper strata material of finally collecting is concentrated, is dried, obtain intermediate product II;
After D.C step, the intermediate product II making is put into the freezing vitriol oil in advance, under condition of ice bath, stir 0.5 hour;
After E.D step, go to immediately under boiling water bath condition, add 5kg gac, stir 1 hour, then filter described gac, collect filtrate crystallisation by cooling, then recrystallization, final drying, obtains.
The purity of the sulfonation dehydroabietic acid that the present embodiment makes is 94.5%.
Embodiment 2
The preparation method of this sulfonation dehydroabietic acid comprises the following steps:
A. under agitation condition, by 65kg nilox resin, 40kg acid clay and 20kg1-methyl-3-octyl group imidazole bisulfate ionic liquid are put into reactor, are uniformly mixed, and then at 105 ℃, reflux 10 hours, obtain intermediate product I;
After B.A step, in described intermediate product I, add 3 times of toluene to extract, collect upper strata material;
After C.B step, repeat B step 2 time, the upper strata material of finally collecting is concentrated, is dried, obtain intermediate product II;
After D.C step, the intermediate product II making is put into the freezing vitriol oil in advance, under condition of ice bath, stir 1 hour;
After E.D step, go to immediately under boiling water bath condition, add 8kg gac, stir 3 hours, then filter described gac, collect filtrate crystallisation by cooling, then recrystallization, final drying, obtains.
The purity of the sulfonation dehydroabietic acid that the present embodiment makes is 95.1%.
Embodiment 3
The preparation method of this sulfonation dehydroabietic acid comprises the following steps:
A. under agitation condition, by 60kg nilox resin, 38kg acid clay and 15kg1-methyl-3-octyl group imidazole bisulfate ionic liquid are put into reactor, are uniformly mixed, and then at 100 ℃, reflux 11 hours, obtain intermediate product I;
After B.A step, in described intermediate product I, add 2 times of toluene to extract, collect upper strata material;
After C.B step, repeat B step 1 time, the upper strata material of finally collecting is concentrated, is dried, obtain intermediate product II;
After D.C step, the intermediate product II making is put into the freezing vitriol oil in advance, under condition of ice bath, stir 0.5 hour;
After E.D step, go to immediately under boiling water bath condition, add 7kg gac, stir 2 hours, then filter described gac, collect filtrate crystallisation by cooling, then recrystallization, final drying, obtains.
The purity of the sulfonation dehydroabietic acid that the present embodiment makes is 95.5%.
Claims (1)
1. a preparation method for sulfonation dehydroabietic acid, is characterized in that comprising the following steps:
A. under agitation condition, by 50 weight part～65 weight part nilox resins, 35 weight part～40 weight part acid clays and 10 weight part～20 weight part 1-methyl-3-octyl group imidazole bisulfate ionic liquids are put into reactor, be uniformly mixed, then at 95 ℃～105 ℃, reflux 10 hours～12 hours, obtain intermediate product I;
After B.A step, in described intermediate product I, add 2 times～3 times toluene to extract, collect upper strata material;
After C.B step, repeat B step 1 time～2 times, by the upper strata material of finally collecting concentrate, dry, obtain intermediate product II;
After D.C step, the intermediate product II making is put into the freezing vitriol oil in advance, under condition of ice bath, stir 0.5 hour～1 hour;
After E.D step, go to immediately under boiling water bath condition, add 5 weight part～8 weight part gacs, stir 1 hour～3 hours, then filter described gac, collect filtrate crystallisation by cooling, then recrystallization, final drying, obtains.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410386057.XA CN104151208A (en) | 2014-08-07 | 2014-08-07 | Preparation method for sulfonated dehydroabietic acid |
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| CN201410386057.XA CN104151208A (en) | 2014-08-07 | 2014-08-07 | Preparation method for sulfonated dehydroabietic acid |
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| CN201410386057.XA Pending CN104151208A (en) | 2014-08-07 | 2014-08-07 | Preparation method for sulfonated dehydroabietic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107628972A (en) * | 2017-10-13 | 2018-01-26 | 重庆康乐制药有限公司 | A kind of sulfur trioxide halohydrocarbon solution sulfonation preparation method of Ecabet |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH083102A (en) * | 1994-06-22 | 1996-01-09 | Harima Chem Inc | Fluorodehydroabietic acid derivative |
| CN1396154A (en) * | 2001-07-16 | 2003-02-12 | 中国医药研究开发中心 | Sulfonated dehydroabietate and its preparing process and application |
| JP2003259891A (en) * | 2002-03-07 | 2003-09-16 | Univ Nihon | Method for producing dehydroabietic acid derivative |
| CN100999487A (en) * | 2006-12-22 | 2007-07-18 | 中国林业科学研究院林产化学工业研究所 | Sulfonated dehydro ferrous abietate, its preparation process and pharmaceutical use |
| CN102659572A (en) * | 2012-04-12 | 2012-09-12 | 浙江工业大学 | Preparation method of dehydroabietic acid |
| CN103896814A (en) * | 2014-01-07 | 2014-07-02 | 珠海亿邦制药股份有限公司 | Method for preparing sulfonated dehydroabietic acid |
-
2014
- 2014-08-07 CN CN201410386057.XA patent/CN104151208A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH083102A (en) * | 1994-06-22 | 1996-01-09 | Harima Chem Inc | Fluorodehydroabietic acid derivative |
| CN1396154A (en) * | 2001-07-16 | 2003-02-12 | 中国医药研究开发中心 | Sulfonated dehydroabietate and its preparing process and application |
| JP2003259891A (en) * | 2002-03-07 | 2003-09-16 | Univ Nihon | Method for producing dehydroabietic acid derivative |
| CN100999487A (en) * | 2006-12-22 | 2007-07-18 | 中国林业科学研究院林产化学工业研究所 | Sulfonated dehydro ferrous abietate, its preparation process and pharmaceutical use |
| CN102659572A (en) * | 2012-04-12 | 2012-09-12 | 浙江工业大学 | Preparation method of dehydroabietic acid |
| CN103896814A (en) * | 2014-01-07 | 2014-07-02 | 珠海亿邦制药股份有限公司 | Method for preparing sulfonated dehydroabietic acid |
Non-Patent Citations (1)
| Title |
|---|
| 刘仕伟等: "酸功能化离子液体磺烷基咪唑对甲苯磺酸盐催化合成松香甲酯的研究", 《林产化学与工业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107628972A (en) * | 2017-10-13 | 2018-01-26 | 重庆康乐制药有限公司 | A kind of sulfur trioxide halohydrocarbon solution sulfonation preparation method of Ecabet |
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Application publication date: 20141119 |