CN104211597B - The preparation method of rosin acid - Google Patents
The preparation method of rosin acid Download PDFInfo
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- CN104211597B CN104211597B CN201410399451.7A CN201410399451A CN104211597B CN 104211597 B CN104211597 B CN 104211597B CN 201410399451 A CN201410399451 A CN 201410399451A CN 104211597 B CN104211597 B CN 104211597B
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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
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- 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 present invention discloses a kind of preparation method of rosin acid, belongs to rosin deep process technology field.The present invention includes and rosin is put into melting still, add dimethylbenzene and turps, oxalic acid and water, stir and melt, cross and filter filter residue, clarification, separation, put into still kettle to distill, rectifying, then put into esterifying kettle, add toxilic acid and glycerine and pimaric acid and carry out esterification, then cool, crystallization, filter, washing, this rosin acid obtained.In the rosin acid that the present invention obtains, the content of pimaric acid reaches more than 95%.
Description
Technical field
The invention belongs to resin field of deep, particularly relate to a kind of preparation method of rosin acid.
Background technology
Rosin is a kind of natural resin, is the physiological metabolism product produced 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, and have fragrance and the bitter taste of pine tree, its main component is resinous acid, lipid acid, unsaponifiables.
Rosin can 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 obtained rosin acid of prior art, the content of pimaric acid is too low, makes 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 obtained rosin acid of prior art, and the content of pimaric acid is too low, makes to act on the problem that can not get well playing.
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 melt still, under agitation, add 3 weight part ~ 5 parts by weight of xylene 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, stir at 60 DEG C ~ 80 DEG C, raw material rosin is melted completely;
After B.A step, cross and filter filter residue, obtain the first fat liquid and 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, recycling design, the residual still liquid obtained, then carry out rectifying, obtained first intermediate product;
After D.C step, first intermediate product is put into esterifying kettle, add 5 weight part ~ 8 parts by weight of maleic and 10 weight part ~ 12 parts by weight of glycerin and 1 weight part ~ 2 weight part pimaric acid, esterification 4 hours ~ 6 hours at 240 DEG C ~ 270 DEG C, obtained second intermediate product;
After E.D step, by the second intermediate product cooling, crystallization, filters, washing, this rosin acid obtained.
Owing to adopting technique scheme, the beneficial effect that the present invention obtains is:
In the rosin acid that the present invention obtains, 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 melt still, under agitation, add 3kg dimethylbenzene and 1kg turps, 0.1kg oxalic acid and 8kg water, stir at 60 DEG C, raw material rosin is melted completely;
After B.A step, cross and filter filter residue, obtain the first fat liquid and 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, recycling design, the residual still liquid obtained, then carry out rectifying, obtained 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, esterification 6 hours at 240 DEG C, obtained second intermediate product;
After E.D step, by the second intermediate product cooling, crystallization, filters, washing, this rosin acid obtained.
In the rosin acid that the present embodiment is obtained, 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 melt still, under agitation, add 5kg dimethylbenzene and 3kg turps, 0.3kg oxalic acid and 12kg water, stir at 80 DEG C, raw material rosin is melted completely;
After B.A step, cross and filter filter residue, obtain the first fat liquid and 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, recycling design, the residual still liquid obtained, then carry out rectifying, obtained 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, esterification 4 hours at 270 DEG C, obtained second intermediate product;
After E.D step, by the second intermediate product cooling, crystallization, filters, washing, this rosin acid obtained.
In the rosin acid that the present embodiment is obtained, 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 melt still, under agitation, add 4kg dimethylbenzene and 2kg turps, 0.2kg oxalic acid and 10kg water, stir at 70 DEG C, raw material rosin is melted completely;
After B.A step, cross and filter filter residue, obtain the first fat liquid and 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, recycling design, the residual still liquid obtained, then carry out rectifying, obtained 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, esterification 5 hours at 2670 DEG C, obtained second intermediate product;
After E.D step, by the second intermediate product cooling, crystallization, filters, washing, this rosin acid obtained.
In the rosin acid that the present embodiment is obtained, 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 melt still, under agitation, add 3 weight part ~ 5 parts by weight of xylene 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, stir at 60 DEG C ~ 80 DEG C, raw material rosin is melted completely;
After B.A step, cross and filter filter residue, obtain the first fat liquid and 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, recycling design, the residual still liquid obtained, then carry out rectifying, obtained first intermediate product;
After D.C step, first intermediate product is put into esterifying kettle, add 5 weight part ~ 8 parts by weight of maleic and 10 weight part ~ 12 parts by weight of glycerin and 1 weight part ~ 2 weight part pimaric acid, esterification 4 hours ~ 6 hours at 240 DEG C ~ 270 DEG C, obtained second intermediate product;
After E.D step, by the second intermediate product cooling, crystallization, filters, washing, this rosin acid obtained.
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 CN104211597A (en) | 2014-12-17 |
| CN104211597B true 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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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105949052A (en) * | 2016-05-26 | 2016-09-21 | 广西众昌树脂有限公司 | Method for producing rosin acid |
| CN105949046A (en) * | 2016-05-26 | 2016-09-21 | 广西众昌树脂有限公司 | Method for preparing 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 |
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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 |
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| CN104211597A (en) | 2014-12-17 |
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