CN104829424A - Method for preparing alpha-terpineol by utilizing turpentine - Google Patents
Method for preparing alpha-terpineol by utilizing turpentine Download PDFInfo
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- CN104829424A CN104829424A CN201510183350.0A CN201510183350A CN104829424A CN 104829424 A CN104829424 A CN 104829424A CN 201510183350 A CN201510183350 A CN 201510183350A CN 104829424 A CN104829424 A CN 104829424A
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- terpineol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/03—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by addition of hydroxy groups to unsaturated carbon-to-carbon bonds, e.g. with the aid of H2O2
- C07C29/04—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by addition of hydroxy groups to unsaturated carbon-to-carbon bonds, e.g. with the aid of H2O2 by hydration of carbon-to-carbon double bonds
- C07C29/05—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by addition of hydroxy groups to unsaturated carbon-to-carbon bonds, e.g. with the aid of H2O2 by hydration of carbon-to-carbon double bonds with formation of absorption products in mineral acids and their hydrolysis
- C07C29/08—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by addition of hydroxy groups to unsaturated carbon-to-carbon bonds, e.g. with the aid of H2O2 by hydration of carbon-to-carbon double bonds with formation of absorption products in mineral acids and their hydrolysis the acid being phosphoric acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
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Abstract
The invention discloses a method for preparing alpha-terpineol by utilizing turpentine and relates to the field of turpentine deep processing technique. According to the technical scheme of the invention, the turpentine is pretreated, purified and fractionated to obtain the oil of turpentine, and then the oil of turpentine is reacted with powdery substances, phosphoric acid, acetic acid and water of 65-75 DEG C to finally obtain alpha-terpineol, wherein the powdery substances are prepared by phosphoric acid and mesoporous gamma alumina in advance. The purity of the above alpha-terpineol is higher than the purity of that prepared through the conventional alpha-terpineol preparation process.
Description
Technical field
The present invention relates to rosin deep process technology field, particularly relate to a kind of method utilizing rosin to prepare alpha-terpineol.
Background technology
The host of alpha-terpineol allotment Syringa oblata Lindl. type essence, alkali resistance is strong, and be applicable to soap compound, its acetic ester has citron and lavender fragrance, for the preparation of essence, also in medicine, agricultural chemicals, plastics, soap, ink, instrument and Electronic Industry.
Turps is the main raw material of alpha-terpineol, and turps can extract from rosin.But due to the terebinthine purity that prior art is obtained not high, cause the purity of the alpha-terpineol obtained with these turps to can not get promoting.
Summary of the invention
The invention provides a kind of method utilizing rosin to prepare alpha-terpineol, the purity of the alpha-terpineol that the method obtains is high, thus can solve the not high purity of the alpha-terpineol obtained with these turps that causes of the terebinthine purity obtained due to prior art and can not get the problem promoted.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
Utilize rosin to prepare a method for alpha-terpineol, the method comprises the following steps:
A, the heating of pending rosin to be melted, then add the turps accounting for described rosin quality 50% ~ 60%, stirs 15 minutes ~ 20 minutes, standing, get supernatant liquid;
B, in the obtained supernatant liquid of step A, first add the carbonic acid of described supernatant liquid quality 0.5% ~ 1%, and stir 30 minutes ~ 60 minutes at 60 DEG C ~ 65 DEG C; And then add 95 DEG C ~ 100 DEG C water accounting for described supernatant liquid quality 15% ~ 18%, stir 40 minutes ~ 50 minutes, leave standstill, get supernatant liquid, obtain clarified resin liquid;
C, clarified resin liquid obtained for step B to be distilled at ambient pressure, collect the cut of 150 DEG C ~ 180 DEG C;
D, by weight, first adds 1 part ~ 5 parts mesoporous gamma alchlors in 10 parts of phosphoric acid, stirs and makes it to dissolve completely, then steams except moisture content and dries, obtaining powdery substance; Again cut, 80 parts ~ 120 parts acetic acid and 50 parts ~ 55 parts 65 DEG C ~ 75 DEG C water that this powdery substance and 1 part ~ 5 parts phosphoric acid, 100 parts of step C obtain are mixed, stir 8 hours ~ 12 hours;
E, material obtained for D step is carried out fractionation, obtain this alpha-terpineol.
In technique scheme, technical scheme is more specifically: in D step, first in 10 parts of phosphoric acid, adds 1 part of mesoporous gamma alchlor, stirs and makes it to dissolve completely, then steams except moisture content and dries, obtaining powdery substance; Again cut, 120 parts of acetic acid and 55 parts of 65 DEG C of water that this powdery substance and 1 part of phosphoric acid, 100 parts of step C obtain are mixed, stir 12 hours.
Further, in D step, first in 10 parts of phosphoric acid, add 5 parts of mesoporous gamma alchlors, stir and make it to dissolve completely, then steam except moisture content and dry, obtaining powdery substance; Again cut, 80 parts of acetic acid and 52 parts of 75 DEG C of water that this powdery substance and 5 parts of phosphoric acid, 100 parts of step C obtain are mixed, stir 8 hours.
Further, in D step, first in 10 parts of phosphoric acid, add 3 parts of mesoporous gamma alchlors, stir and make it to dissolve completely, then steam except moisture content and dry, obtaining powdery substance; Again cut, 100 parts of acetic acid and 50 parts of 70 DEG C of water that this powdery substance and 3 parts of phosphoric acid, 100 parts of step C obtain are mixed, stir 10 hours.
Owing to adopting technique scheme, the present invention has following beneficial effect:
The present invention is by first carrying out pre-treatment, purification, fractionation by rosin, obtain turps, and then react with prior powdery substance, phosphoric acid, acetic acid and 65 DEG C ~ 75 DEG C water one obtained by phosphoric acid and mesoporous gamma alchlor, the purity of the alpha-terpineol finally making the purity of the alpha-terpineol obtained obtain than alpha-terpineol preparation technology is in the past high.
Embodiment
Below in conjunction with specific examples, the invention will be further described:
Embodiment 1
The method utilizing rosin to prepare alpha-terpineol comprises the following steps:
A, the heating of pending rosin to be melted, then add the turps accounting for described rosin quality 50%, stirs 15 minutes, standing, get supernatant liquid;
B, in the obtained supernatant liquid of step A, first add the carbonic acid of described supernatant liquid quality 0.5%, and stir 30 minutes at 60 DEG C; And then add the 95 DEG C of water accounting for described supernatant liquid quality 15%, stir 40 minutes, leave standstill, get supernatant liquid, obtain clarified resin liquid;
C, clarified resin liquid obtained for step B to be distilled at ambient pressure, collect the cut of 150 DEG C ~ 180 DEG C;
D, by weight, first adds 1 part of mesoporous gamma alchlor in 10 parts of phosphoric acid, stirs and makes it to dissolve completely, then steams except moisture content and dries, obtaining powdery substance; Again cut, 120 parts of acetic acid and 55 parts of 65 DEG C of water that this powdery substance and 1 part of phosphoric acid, 100 parts of step C obtain are mixed, stir 12 hours;
E, material obtained for D step is carried out fractionation, obtain the alpha-terpineol that purity is 99.4%.
Embodiment 2
The method utilizing rosin to prepare alpha-terpineol comprises the following steps:
A, the heating of pending rosin to be melted, then add the turps accounting for described rosin quality 60%, stirs 20 minutes, standing, get supernatant liquid;
B, in the obtained supernatant liquid of step A, first add the carbonic acid of described supernatant liquid quality 1%, and stir 60 minutes at 65 DEG C; And then add the 100 DEG C of water accounting for described supernatant liquid quality 18%, stir 50 minutes, leave standstill, get supernatant liquid, obtain clarified resin liquid;
C, clarified resin liquid obtained for step B to be distilled at ambient pressure, collect the cut of 150 DEG C ~ 180 DEG C;
D, by weight, in D step, first adds 5 parts of mesoporous gamma alchlors, stirs and make it to dissolve completely in 10 parts of phosphoric acid, then steams except moisture content and dries, obtaining powdery substance; Again cut, 80 parts of acetic acid and 52 parts of 75 DEG C of water that this powdery substance and 5 parts of phosphoric acid, 100 parts of step C obtain are mixed, stir 8 hours;
E, material obtained for D step is carried out fractionation, obtain the alpha-terpineol that purity is 99.6%.
Embodiment 3
The method utilizing rosin to prepare alpha-terpineol comprises the following steps:
A, the heating of pending rosin to be melted, then add the turps accounting for described rosin quality 55%, stirs 18 minutes, standing, get supernatant liquid;
B, in the obtained supernatant liquid of step A, first add the carbonic acid of described supernatant liquid quality 0.8%, and stir 45 minutes at 62 DEG C; And then add the 98 DEG C of water accounting for described supernatant liquid quality 16%, stir 45 minutes, leave standstill, get supernatant liquid, obtain clarified resin liquid;
C, clarified resin liquid obtained for step B to be distilled at ambient pressure, collect the cut of 150 DEG C ~ 180 DEG C;
D, by weight, first adds 3 parts of mesoporous gamma alchlors in 10 parts of phosphoric acid, stirs and makes it to dissolve completely, then steams except moisture content and dries, obtaining powdery substance; Again cut, 100 parts of acetic acid and 50 parts of 70 DEG C of water that this powdery substance and 3 parts of phosphoric acid, 100 parts of step C obtain are mixed, stir 10 hours;
E, material obtained for D step is carried out fractionation, obtain the alpha-terpineol that purity is 99.5%.
Claims (4)
1. utilize rosin to prepare a method for alpha-terpineol, it is characterized in that its preparation process is as follows:
A, the heating of pending rosin to be melted, then add the turps accounting for described rosin quality 50% ~ 60%, stirs 15 minutes ~ 20 minutes, standing, get supernatant liquid;
B, in the obtained supernatant liquid of step A, first add the carbonic acid of described supernatant liquid quality 0.5% ~ 1%, and stir 30 minutes ~ 60 minutes at 60 DEG C ~ 65 DEG C; And then add 95 DEG C ~ 100 DEG C water accounting for described supernatant liquid quality 15% ~ 18%, stir 40 minutes ~ 50 minutes, leave standstill, get supernatant liquid, obtain clarified resin liquid;
C, clarified resin liquid obtained for step B to be distilled at ambient pressure, collect the cut of 150 DEG C ~ 180 DEG C;
D, by weight, first adds 1 part ~ 5 parts mesoporous gamma alchlors in 10 parts of phosphoric acid, stirs and makes it to dissolve completely, then steams except moisture content and dries, obtaining powdery substance; Cut, 80 parts ~ 120 parts acetic acid and 50 parts ~ 55 parts 65 DEG C ~ 75 DEG C water that this powdery substance and 1 part ~ 5 parts phosphoric acid, 100 parts of step C obtain are mixed, stirs 8 hours ~ 12 hours;
E, material obtained for D step is carried out fractionation, obtain this alpha-terpineol.
2. the method utilizing rosin to prepare alpha-terpineol according to claim 1, is characterized in that: in D step, first in 10 parts of phosphoric acid, adds 1 part of mesoporous gamma alchlor, stirs and makes it to dissolve completely, then steams except moisture content and dries, obtaining powdery substance; Cut, 120 parts of acetic acid and 55 parts of 65 DEG C of water that this powdery substance and 1 part of phosphoric acid, 100 parts of step C obtain are mixed, stirs 12 hours.
3. the method utilizing rosin to prepare alpha-terpineol according to claim 1, is characterized in that: in D step, first in 10 parts of phosphoric acid, adds 5 parts of mesoporous gamma alchlors, stirs and makes it to dissolve completely, then steams except moisture content and dries, obtaining powdery substance; Cut, 80 parts of acetic acid and 52 parts of 75 DEG C of water that this powdery substance and 5 parts of phosphoric acid, 100 parts of step C obtain are mixed, stirs 8 hours.
4. the method utilizing rosin to prepare alpha-terpineol according to claim 1, is characterized in that: in D step, first in 10 parts of phosphoric acid, adds 3 parts of mesoporous gamma alchlors, stirs and makes it to dissolve completely, then steams except moisture content and dries, obtaining powdery substance; Again cut, 100 parts of acetic acid and 50 parts of 70 DEG C of water that this powdery substance and 3 parts of phosphoric acid, 100 parts of step C obtain are mixed, stir 10 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510183350.0A CN104829424A (en) | 2015-04-17 | 2015-04-17 | Method for preparing alpha-terpineol by utilizing turpentine |
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| CN201510183350.0A CN104829424A (en) | 2015-04-17 | 2015-04-17 | Method for preparing alpha-terpineol by utilizing turpentine |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4111900A1 (en) * | 1991-04-12 | 1992-10-15 | Haarmann & Reimer Gmbh | Optically active alpha-terpineol prodn. - by hydration of optically active alpha- and/or beta-pinene using specified acid mixt. |
| CN101108788A (en) * | 2007-07-13 | 2008-01-23 | 中国林业科学研究院林产化学工业研究所 | Method of manufacturing high purity alpha-terpineol |
| CN102276420A (en) * | 2011-06-22 | 2011-12-14 | 中国林业科学研究院林产化学工业研究所 | Process of preparing terpineol |
| CN102627528A (en) * | 2012-03-16 | 2012-08-08 | 云南森美达生物科技有限公司 | Method for synthesis of terpineol by supersonic wave assistance |
| US20140121148A1 (en) * | 2011-06-09 | 2014-05-01 | Richard Winget | Restoration and preservation formulation for polymeric products |
| CN103787835A (en) * | 2014-02-18 | 2014-05-14 | 广东森宇林产化工有限公司 | Process for preparing terpilenol |
-
2015
- 2015-04-17 CN CN201510183350.0A patent/CN104829424A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4111900A1 (en) * | 1991-04-12 | 1992-10-15 | Haarmann & Reimer Gmbh | Optically active alpha-terpineol prodn. - by hydration of optically active alpha- and/or beta-pinene using specified acid mixt. |
| CN101108788A (en) * | 2007-07-13 | 2008-01-23 | 中国林业科学研究院林产化学工业研究所 | Method of manufacturing high purity alpha-terpineol |
| US20140121148A1 (en) * | 2011-06-09 | 2014-05-01 | Richard Winget | Restoration and preservation formulation for polymeric products |
| CN102276420A (en) * | 2011-06-22 | 2011-12-14 | 中国林业科学研究院林产化学工业研究所 | Process of preparing terpineol |
| CN102627528A (en) * | 2012-03-16 | 2012-08-08 | 云南森美达生物科技有限公司 | Method for synthesis of terpineol by supersonic wave assistance |
| CN103787835A (en) * | 2014-02-18 | 2014-05-14 | 广东森宇林产化工有限公司 | Process for preparing terpilenol |
Non-Patent Citations (1)
| Title |
|---|
| 唐玉章: "松香和松节油的加工技术", 《生意通》 * |
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Application publication date: 20150812 |