CN102634282A - Novel method for softening rosin - Google Patents
Novel method for softening rosin Download PDFInfo
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- CN102634282A CN102634282A CN201210098901XA CN201210098901A CN102634282A CN 102634282 A CN102634282 A CN 102634282A CN 201210098901X A CN201210098901X A CN 201210098901XA CN 201210098901 A CN201210098901 A CN 201210098901A CN 102634282 A CN102634282 A CN 102634282A
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Abstract
The invention discloses a novel method for softening rosin, which includes: using a byproduct, namely turpentine, pinene or petroleum ether produced by rosin softening enterprises as solvent, and obtaining high-acidity high quality rosin with first-class color degree by thermal filtering, decomposed leaching or press filtering, and crystalizing. The solvent is directly recyclable, so that production energy consumption is low, and production cost is reduced effectively. The method has the advantages that the rosin softened is light in color and high in yield, the solvent used is low in toxicity, heating time is short, energy consumption is low, production cost is reduced effectively and operation is simple, and the method is easy for industrial production and especially applicable to purification of high-acidity high quality rosins in light color.
Description
Technical field
The present invention relates to the rosin purification process, especially relate to a kind of rosiny rosin purifying novel method of from rosin, refining.
Background technology
Rosin is a kind of abundant renewable natural industrial chemicals of originating, and it is described as " lignicolous oil ".According to statistics, rosin and turps have 400 multiple uses, are important industrial raw material, can be widely used in industry such as soap, papermaking, rubber, coating, chemical industry, medicine, food, plastics, electrician, agricultural chemicals, printing.Along with industrial production and science and technology development, to the increase year by year of rosin and turps demand.China is as rosin big producing country, and the YO of ester rosin ranks first in the world more than 500,000 tons.Simultaneously, rosin also is one of traditional large exporting of China.
The rosiny staple is the various resinous acids with one three luxuriant and rich with fragrance skeleton structure of ring; Be broadly divided into abietic type acid, Korean pine type resinous acid and three main types of other resinous acid; Also have little fat acid and nonacid material simultaneously, and coloring matter such as resene acid.Coloring matters such as nonacid material and resene acid can influence rosiny exterior quality and use properties.No matter be direct use, deep processing or synthetic fine chemicals, generally all need coloring matter, unsaponifiable matter, lipid acid and other impurity be wherein removed.Therefore, improve the rosiny purification process, reduce environmental pollution and production cost, obtain the high-quality significant and good economic benefit of pale rosin.
At present; The method relatively more commonly used to the rosiny refinement treatment mainly contains: (1) utilizes rosiny acid and mineral alkali or water-soluble ammonium salt or the sodium salt of organic bases generation chemical reaction generation; And neutral substance does not react, thereby neutral unsaponifiables is separated.Gained ammonium salt or sodium salt are acidified again, extracting and separating obtains the high rosin of resinous acid content.Yet the chemical reagent consumption of this method is big, can produce great amount of wastewater, and the separating technology difficulty is big, is unfavorable for suitability for industrialized production.(2) under the condition of not destroying the rosin staple, incite somebody to action Impurity removal wherein through means such as the use of distillation, SX, absorption, washing, phenol and the uses of polyvalent alcohol.Simple owing to distillation method technology, be easy to continuous large-scale production and be widely used.But temperature that this manipulation require is higher and higher vacuum condition are therefore higher to equipment requirements, investment is bigger, and energy consumption is also high in addition.In patent (CN200910114433.9), utilize the difference of the solubleness of Gum Rosin in methylene dichloride and acetonitrile to purify, but two kinds of solvents that this method is used all have bigger toxicity, are prone to cause environmental pollution, cost is higher.
Summary of the invention
The object of the present invention is to provide a kind of rosin purifying novel method low, that energy consumption is low of polluting, the solvent that this method is selected for use and reclaimed easily, pollution is low, cost is low, thereby make things convenient for recycling.
The objective of the invention is to realize like this:
A kind of rosin purifying novel method, characteristic is: may further comprise the steps:
1, Gum Rosin is put into container, add the organic solvent of low toxicity again, heating for dissolving, the temperature of heating for dissolving is 80-200 ℃, after stirring, heat filtering is removed wood chip and earth insoluble impurities, obtains first-time filtrate;
2, with first-time filtrate be-30-30 ℃ cooling down at cooling temperature; Left standstill 10 minutes to 10 hours; Rosin acid is fully separated out, and crystallization obtains the high-quality finished colophonium that acid number height, color and luster degree reach one-level, passes through decompress filter or press filtration then; Obtain rosin acid filter cake and secondary filtrating respectively, secondary filtrating is reclaimed obtain turps;
3,, promptly get the high-quality finished colophonium that acid number is high, the color and luster degree reaches one-level behind the cooling curing with rosin acid filter cake normal pressure heat fused under protection of inert gas of gained.
Organic solvent described in the step 1 is turps, firpene or sherwood oil, preferred especially turps; The massfraction that described organic solvent accounts for Gum Rosin is 20%～70%.
In step 1, secondary filtrating is directly reclaimed and is obtained turps or reclaim firpene or sherwood oil through distillation.
Rare gas element described in the step 3 is nitrogen, argon gas or carbonic acid gas, special nitrogen.
The sub product of 3 the present invention through selecting for use rosin processing enterprise self to produce: turps, firpene or sherwood oil be as solvent, through obtaining the high-quality rosin that acid number height, color and luster degree reach one-level after heat filtering, decompress filter or press filtration, the crystallization.Organic solvent is recovery set usefulness directly, makes that the production energy consumption is low, effectively reduces production costs.The present invention has that gained rosin product colour is very shallow, yield is high, the solvent for use low toxicity, heat-up time is short, energy consumption is low, effectively reduce production costs, advantage simple to operate; Be easy to suitability for industrialized production, be specially adapted to light color, high-quality rosiny purifying that acid number is high.
Embodiment
Below in conjunction with embodiment the present invention is done further explain.
Embodiment 1:
With adding in the 100mL Erlenmeyer flask behind the 35 gram Pinus massoniana Lamb rosin porphyrizes, add 30mL turps again, be warmed up to 100 ℃ after, Pinus massoniana Lamb rosin dissolves fully, heat filtering is removed wood chip and earth insoluble impurities, obtains first-time filtrate.First-time filtrate slowly is cooled to 20 ℃, and rosin acid is fully separated out, and crystallization obtains refined light-color rosin, passes through decompress filter then, obtains rosin acid filter cake and secondary filtrating respectively, and secondary filtrating is reclaimed and obtained turps.With resinous acid filter cake normal pressure heat fused under protection of nitrogen gas of gained, cooling curing obtains refined light-color rosin.
Embodiment 2:
110 gram slash pine rosin are added in the 250mL Erlenmeyer flasks, add 30mL turps again, be warmed up to 200 ℃ after, slash pine rosin dissolves fully, heat filtering is removed wood chip and earth insoluble impurities, obtains first-time filtrate.First-time filtrate slowly is cooled to 30 ℃, and rosin acid is fully separated out, and crystallization obtains refined light-color rosin, passes through press filtration then, obtains rosin acid filter cake and secondary filtrating respectively, and secondary filtrating is reclaimed and obtained turps.With resinous acid filter cake normal pressure heat fused under protection of nitrogen gas of gained, cooling curing obtains refined light-color rosin.
Embodiment 3:
With adding in the 250mL Erlenmeyer flask behind the 100 gram Pinus massoniana Lamb rosin porphyrizes, add 70mL turps again, be warmed up to 110 ℃ after, the dissolving of Pinus massoniana Lamb rosin fully, heat filtering is removed wood chip and earth insoluble impurities, obtains first-time filtrate.First-time filtrate slowly is cooled to 25 ℃, and rosin acid is fully separated out, and crystallization obtains refined light-color rosin, passes through decompress filter then, obtains rosin acid filter cake and secondary filtrating respectively, and secondary filtrating is reclaimed and obtained turps.With resinous acid filter cake normal pressure heat fused under the protection of argon gas of gained, cooling curing obtains refined light-color rosin.
Embodiment 4:
With adding in the 500mL Erlenmeyer flask behind the 300 gram Pinus massoniana Lamb rosin porphyrizes, add 90mL turps again, be warmed up to 160 ℃ after, the dissolving of Pinus massoniana Lamb rosin fully, heat filtering is removed wood chip and earth insoluble impurities, obtains first-time filtrate.First-time filtrate slowly is cooled to 0 ℃, and rosin acid is fully separated out, and crystallization obtains refined light-color rosin, passes through decompress filter then, obtains rosin acid filter cake and secondary filtrating respectively, and secondary filtrating is reclaimed and obtained turps.With resinous acid filter cake normal pressure heat fused under protection of nitrogen gas of gained, cooling curing obtains refined light-color rosin.
Embodiment 5:
With adding in the 500mL Erlenmeyer flask behind the 510 gram slash pine rosin porphyrizes, add the 60mL firpene again, be warmed up to 130 ℃ after, the dissolving of slash pine rosin fully, heat filtering is removed wood chip and earth insoluble impurities, obtains first-time filtrate.First-time filtrate slowly is cooled to-25 ℃, and rosin acid is fully separated out, and crystallization obtains refined light-color rosin, passes through decompress filter then, obtains rosin acid filter cake and secondary filtrating respectively, and secondary filtrating is reclaimed and obtained turps.With resinous acid filter cake normal pressure heat fused under the protection of carbonic acid gas of gained, cooling curing obtains refined light-color rosin.
Embodiment 6:
With adding in the 250mL Erlenmeyer flask behind the 100 gram Pinus massoniana Lamb rosin porphyrizes, add the 40mL sherwood oil again, be warmed up to 80 ℃ after, the dissolving of Pinus massoniana Lamb rosin fully, heat filtering is removed wood chip and earth insoluble impurities, obtains first-time filtrate.First-time filtrate slowly is cooled to-5 ℃, and rosin acid is fully separated out, and crystallization obtains refined light-color rosin, and decompress filter obtains rosin acid filter cake and secondary filtrating respectively then, and secondary filtrating is reclaimed and obtained turps.With resinous acid filter cake normal pressure heat fused under protection of nitrogen gas of gained, cooling curing obtains refined light-color rosin.
Claims (6)
1. rosin purifying novel method is characterized in that:
(1), Gum Rosin is put into container, add the organic solvent of low toxicity again, heating for dissolving, the temperature of heating for dissolving is 80-200 ℃, after stirring, heat filtering is removed wood chip and earth insoluble impurities, obtains first-time filtrate;
(2), with first-time filtrate be-30-30 ℃ cooling down at cooling temperature; Left standstill 10 minutes to 10 hours; Rosin acid is fully separated out, and crystallization obtains the high-quality finished colophonium that acid number height, color and luster degree reach one-level, passes through decompress filter or press filtration then; Obtain rosin acid filter cake and secondary filtrating respectively, secondary filtrating is reclaimed obtain turps;
(3), with rosin acid filter cake normal pressure heat fused under protection of inert gas of gained, promptly get the high-quality finished colophonium that acid number is high, the color and luster degree reaches one-level behind the cooling curing.
2. rosin purifying novel method according to claim 1 is characterized in that: the organic solvent described in the step 1 is turps, firpene or sherwood oil, and the massfraction that described organic solvent accounts for Gum Rosin is 20%～70%.
3. rosin purifying novel method according to claim 2 is characterized in that: the preferred turps of described organic solvent.
4. rosin purifying novel method according to claim 1 is characterized in that: in step 1, secondary filtrating is directly reclaimed and is obtained turps or reclaim firpene or sherwood oil through distillation.
5. rosin purifying novel method according to claim 1 is characterized in that: the rare gas element described in the step 3 is nitrogen, argon gas or carbonic acid gas.
6. rosin purifying novel method according to claim 5 is characterized in that: the rare gas element nitrogen described in the step 3.
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| CN201210098901XA CN102634282A (en) | 2012-04-06 | 2012-04-06 | Novel method for softening rosin |
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| CN201210098901XA CN102634282A (en) | 2012-04-06 | 2012-04-06 | Novel method for softening rosin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211596A (en) * | 2014-08-14 | 2014-12-17 | 广西众昌树脂有限公司 | Preparation method of rosin acid |
| CN104211597A (en) * | 2014-08-14 | 2014-12-17 | 广西众昌树脂有限公司 | Preparation method of rosin acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4643847A (en) * | 1985-11-12 | 1987-02-17 | Hercules Incorporated | Method of improving the color of tall oil rosin |
| CN1613940A (en) * | 2004-09-27 | 2005-05-11 | 广西大学 | Water-white hydrogenating rosin production |
| CN101362924A (en) * | 2008-10-08 | 2009-02-11 | 中国林业科学研究院林产化学工业研究所 | Method for decolorization preparation of pale rosin by rosin containing non-decoloring agent |
-
2012
- 2012-04-06 CN CN201210098901XA patent/CN102634282A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4643847A (en) * | 1985-11-12 | 1987-02-17 | Hercules Incorporated | Method of improving the color of tall oil rosin |
| CN1613940A (en) * | 2004-09-27 | 2005-05-11 | 广西大学 | Water-white hydrogenating rosin production |
| CN101362924A (en) * | 2008-10-08 | 2009-02-11 | 中国林业科学研究院林产化学工业研究所 | Method for decolorization preparation of pale rosin by rosin containing non-decoloring agent |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211596A (en) * | 2014-08-14 | 2014-12-17 | 广西众昌树脂有限公司 | Preparation method of rosin acid |
| CN104211597A (en) * | 2014-08-14 | 2014-12-17 | 广西众昌树脂有限公司 | Preparation method of rosin acid |
| CN104211596B (en) * | 2014-08-14 | 2016-03-09 | 广西众昌树脂有限公司 | The preparation method of rosin acid |
| CN104211597B (en) * | 2014-08-14 | 2016-03-09 | 广西众昌树脂有限公司 | The preparation method of rosin acid |
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Application publication date: 20120815 |