CN104211597A - Preparation method of rosin acid - Google Patents
Preparation method of rosin acid Download PDFInfo
- Publication number
- CN104211597A CN104211597A CN201410399451.7A CN201410399451A CN104211597A CN 104211597 A CN104211597 A CN 104211597A CN 201410399451 A CN201410399451 A CN 201410399451A CN 104211597 A CN104211597 A CN 104211597A
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- weight part
- acid
- rosin
- intermediate product
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/487—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
- C07C51/493—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification whereby carboxylic acid esters are formed
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2603/00—Systems containing at least three condensed rings
- C07C2603/02—Ortho- or ortho- and peri-condensed systems
- C07C2603/04—Ortho- or ortho- and peri-condensed systems containing three rings
- C07C2603/22—Ortho- or ortho- and peri-condensed systems containing three rings containing only six-membered rings
- C07C2603/26—Phenanthrenes; Hydrogenated phenanthrenes
Abstract
The invention discloses a preparation method of rosin acid, and belongs to the technical field of deep processing of rosin. The method comprises the following steps: putting turpentine in a melting kettle, adding xylene, turpentine oil, oxalic acid and water, carrying out stirring melting, filtering to remove filter residues, clarifying, separating, distilling in a distillation kettle, rectifying, putting the above obtained rectified material in an esterification kettle, adding maleic acid, glycerin and pimaric acid, carrying out an esterification reaction, cooling, crystallizing, filtering, and washing to prepare the rosin acid. The content of pimaric acid in the rosin acid prepared in the invention reaches above 95%.
Description
Technical field
The invention belongs to resin deep processing field, relate in particular to a kind of preparation method of rosin acid.
Background technology
Rosin is a kind of natural resin, is the physiological metabolism product producing in pine genus tree vital movement process, is a kind of oil-containing natural resin, is colourless, transparent viscous liquid.Rosin is mainly gathered in the pine resin road of pine tree, has fragrance and the bitter taste of pine tree, and its main component is resinous acid, lipid acid, unsaponifiables.
Rosin can be by being processed into rosin acid, and the main component of rosin acid is abietic acid, pimaric acid, palustric acid, neoabietic acid, and wherein, pimaric acid all has purposes widely at medicine, agricultural chemicals, tensio-active agent, chiral catalyst etc.But in the rosin acid that prior art makes, the content of pimaric acid is too low, make effect can not get good performance.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of preparation method of rosin acid, and the method can solve in the rosin acid that prior art makes, and the content of pimaric acid is too low, make effect can not get the well problem of performance.
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. 30 weight part～45 weight part rosin are put into and melted still, under agitation condition, add 3 weight part～5 weight part dimethylbenzene and 1 weight part～3 weight part turps, 0.1 weight part～0.3 weight part oxalic acid and 8 weight part～12 weight parts waters, at 60 DEG C～80 DEG C, stir, raw material fallen rosin is melted completely;
After B.A step, remove by filter filter residue, obtain the first fat liquid and will put into clarifying kettle, clarification, separation obtain the second fat liquid;
After C.B step, the second fat liquid is put into still kettle, 150 DEG C～180 DEG C distillations 1 hour～3 hours, reclaim solvent, the residual still liquid obtaining, then carry out rectifying, make the first intermediate product;
After D.C step, the first intermediate product is put into esterifying kettle, add 5 weight part～8 weight part toxilic acids and 10 weight part～12 weight part glycerine and 1 weight part～2 weight part pimaric acid, at 240 DEG C～270 DEG C, esterification 4 hours～6 hours, makes the second intermediate product;
After E.D step, by cooling the second intermediate product, crystallization, filters, and washing, makes this rosin acid.
Owing to adopting technique scheme, the beneficial effect that the present invention obtains is:
In the rosin acid that the present invention makes, the content of pimaric acid reaches more than 95%.
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 rosin acid comprises the following steps:
A. 30kg rosin is put into and melted still, under agitation condition, add 3kg dimethylbenzene and 1kg turps, 0.1kg oxalic acid and 8kg water stir at 60 DEG C, and raw material fallen rosin is melted completely;
After B.A step, remove by filter filter residue, obtain the first fat liquid and will put into clarifying kettle, clarification, separation obtain the second fat liquid;
After C.B step, the second fat liquid is put into still kettle, 150 DEG C of distillations 3 hours, reclaim solvent, the residual still liquid obtaining, then carry out rectifying, make the first intermediate product;
After D.C step, the first intermediate product is put into esterifying kettle, add 5kg toxilic acid and 10kg glycerine and 1kg pimaric acid, at 240 DEG C, esterification 6 hours, makes the second intermediate product;
After E.D step, by cooling the second intermediate product, crystallization, filters, and washing, makes this rosin acid.
In the rosin acid that the present embodiment makes, the content of pimaric acid is 95%.
Embodiment 2
The preparation method of this rosin acid comprises the following steps:
A. 45kg rosin is put into and melted still, under agitation condition, add 5kg dimethylbenzene and 3kg turps, 0.3kg oxalic acid and 12kg water, stir at 80 DEG C, and raw material fallen rosin is melted completely;
After B.A step, remove by filter filter residue, obtain the first fat liquid and will put into clarifying kettle, clarification, separation obtain the second fat liquid;
After C.B step, the second fat liquid is put into still kettle, 180 DEG C of distillations 1 hour, reclaim solvent, the residual still liquid obtaining, then carry out rectifying, make the first intermediate product;
After D.C step, the first intermediate product is put into esterifying kettle, add 8kg toxilic acid and 12kg glycerine and 2kg pimaric acid, at 270 DEG C, esterification 4 hours, makes the second intermediate product;
After E.D step, by cooling the second intermediate product, crystallization, filters, and washing, makes this rosin acid.
In the rosin acid that the present embodiment makes, the content of pimaric acid is 96.5%.
Embodiment 3
The preparation method of this rosin acid comprises the following steps:
A. 40kg rosin is put into and melted still, under agitation condition, add 4kg dimethylbenzene and 2kg turps, 0.2kg oxalic acid and 10kg water stir at 70 DEG C, and raw material fallen rosin is melted completely;
After B.A step, remove by filter filter residue, obtain the first fat liquid and will put into clarifying kettle, clarification, separation obtain the second fat liquid;
After C.B step, the second fat liquid is put into still kettle, 160 DEG C of distillations 2 hours, reclaim solvent, the residual still liquid obtaining, then carry out rectifying, make the first intermediate product;
After D.C step, the first intermediate product is put into esterifying kettle, add 6kg toxilic acid and 11kg glycerine and 1.5kg pimaric acid, at 2670 DEG C, esterification 5 hours, makes the second intermediate product;
After E.D step, by cooling the second intermediate product, crystallization, filters, and washing, makes this rosin acid.
In the rosin acid that the present embodiment makes, the content of pimaric acid is 96%.
Claims (1)
1. a preparation method for rosin acid, is characterized in that comprising the following steps:
A. 30 weight part～45 weight part rosin are put into and melted still, under agitation condition, add 3 weight part～5 weight part dimethylbenzene and 1 weight part～3 weight part turps, 0.1 weight part～0.3 weight part oxalic acid and 8 weight part～12 weight parts waters, at 60 DEG C～80 DEG C, stir, raw material fallen rosin is melted completely;
After B.A step, remove by filter filter residue, obtain the first fat liquid and will put into clarifying kettle, clarification, separation obtain the second fat liquid;
After C.B step, the second fat liquid is put into still kettle, 150 DEG C～180 DEG C distillations 1 hour～3 hours, reclaim solvent, the residual still liquid obtaining, then carry out rectifying, make the first intermediate product;
After D.C step, the first intermediate product is put into esterifying kettle, add 5 weight part～8 weight part toxilic acids and 10 weight part～12 weight part glycerine and 1 weight part～2 weight part pimaric acid, at 240 DEG C～270 DEG C, esterification 4 hours～6 hours, makes the second intermediate product;
After E.D step, by cooling the second intermediate product, crystallization, filters, and washing, makes this rosin acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410399451.7A CN104211597B (en) | 2014-08-14 | 2014-08-14 | The preparation method of rosin acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410399451.7A CN104211597B (en) | 2014-08-14 | 2014-08-14 | The preparation method of rosin acid |
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| Publication Number | Publication Date |
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| CN104211597A true CN104211597A (en) | 2014-12-17 |
| CN104211597B CN104211597B (en) | 2016-03-09 |
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| CN201410399451.7A Active CN104211597B (en) | 2014-08-14 | 2014-08-14 | The preparation method of rosin acid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105949046A (en) * | 2016-05-26 | 2016-09-21 | 广西众昌树脂有限公司 | Method for preparing rosin acid |
| CN105949052A (en) * | 2016-05-26 | 2016-09-21 | 广西众昌树脂有限公司 | Method for producing rosin acid |
| CN106047180A (en) * | 2016-06-29 | 2016-10-26 | 潘宇 | Preparation method of high-softening-point rosin |
| CN106336353A (en) * | 2016-08-29 | 2017-01-18 | 广西梧州通轩林产化学有限公司 | Preparation method of abietic resin acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634282A (en) * | 2012-04-06 | 2012-08-15 | 井冈山大学 | Novel method for softening rosin |
| CN103360952A (en) * | 2012-04-06 | 2013-10-23 | 广西众昌树脂有限公司 | Special modified rosin resin for road marking paint and preparation method of special modified rosin resin |
| CN103484023A (en) * | 2013-08-29 | 2014-01-01 | 四会市邦得利化工有限公司 | Method for preparing polyol ester resin of terpene and rosin diene addition product from rosin |
-
2014
- 2014-08-14 CN CN201410399451.7A patent/CN104211597B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634282A (en) * | 2012-04-06 | 2012-08-15 | 井冈山大学 | Novel method for softening rosin |
| CN103360952A (en) * | 2012-04-06 | 2013-10-23 | 广西众昌树脂有限公司 | Special modified rosin resin for road marking paint and preparation method of special modified rosin resin |
| CN103484023A (en) * | 2013-08-29 | 2014-01-01 | 四会市邦得利化工有限公司 | Method for preparing polyol ester resin of terpene and rosin diene addition product from rosin |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105949046A (en) * | 2016-05-26 | 2016-09-21 | 广西众昌树脂有限公司 | Method for preparing rosin acid |
| CN105949052A (en) * | 2016-05-26 | 2016-09-21 | 广西众昌树脂有限公司 | Method for producing rosin acid |
| CN106047180A (en) * | 2016-06-29 | 2016-10-26 | 潘宇 | Preparation method of high-softening-point rosin |
| CN106336353A (en) * | 2016-08-29 | 2017-01-18 | 广西梧州通轩林产化学有限公司 | Preparation method of abietic resin acid |
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| Publication number | Publication date |
|---|---|
| CN104211597B (en) | 2016-03-09 |
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