CN103232816A - Preparation method of rosin - Google Patents
Preparation method of rosin Download PDFInfo
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- CN103232816A CN103232816A CN2013101640960A CN201310164096A CN103232816A CN 103232816 A CN103232816 A CN 103232816A CN 2013101640960 A CN2013101640960 A CN 2013101640960A CN 201310164096 A CN201310164096 A CN 201310164096A CN 103232816 A CN103232816 A CN 103232816A
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Abstract
The invention discloses a preparation method of rosin. The preparation method comprises the following steps of: step 1, dissolving rosin in a benign solvent and filtering to remove insoluble impurities, adding a non-benign solvent while stirring, standing for 1-10 hours under normal temperature, filtering and colleting precipitates; step 2, heating and carrying out isomerization treatment on all precipitates for 1-3 hours under the protection of N2 or CO2 at 150 DEG C to 180 DEG C, and cooling; and step 3, filling the prepared rough rosin to a sealed container, heating up to 250 DEG C to 265 DEG C, collecting fractions, condensing and storing; increasing the temperature to 270 DEG C to 280 DEG C, so that the rosin is changed into a gaseous state from a liquid state, cooling to 230 DEG C to 250 DEG C, so that the rosin is changed into the liquid state from the gaseous state, transferring the liquid rosin to a reaction container, adding a rosin decolorizing agent, heating up to 270 DEG C under stirring, slowly cooling to 180 DEG C to 220 DEG C, adding a rosin stabilizing agent, cooling to 90 DEG C to 120 DEG C, discharging and packaging or pelletizing by a pelletizer. According to the preparation method of the rosin, the prepared rosin is free of a pungent smell, almost transparent and colorless in appearance and stable in quality.
Description
Technical field
The present invention relates to a kind of preparation method of rosin, particularly, relate to a kind of preparation method of light odorlessness rosin.
Background technology
Rosin is a kind of complex mixture that makes from rosin, pine torch or tall oil, hard and crisp, is generally yellow or brown, as industrial raw material.Rosin mainly is made up of various diterpenoid resin acids, also contains little fat acid and neutrals, and its amount press rosin kind difference and different.
Rosin is divided into 3 kinds of gum resin, wood rosin, starex by its source.Gum resin also claims to loosen perfume (or spice), and is of light color, and acid number is big, the softening temperature height; Wood rosin claims steam distilled rosin again, and quality is not as gum resin, and color is dark, and acid number is little, and easily crystallization from some solvent; Starex claims toll oil rosin again.Rosin is the solid natural resin of two kinds of transparent, fragility, is the mixture of more complicated, is made up of resinous acid (abietic acid, pimaric acid), little fat acid, rosin acid anhydrides and neutrals etc.The main component of rosin is resinous acid, accounts for about 90%, and molecular formula is C
19H
29-COOH, molecular weight 302.46.Resinous acid is most representative sylvic acid, belongs to unsaturated acid, contains conjugated double bond, and the strong absorption UV-light can autoxidation in air or induce rear oxidation.The rosin outward appearance is faint yellow to light brown, and glassy gloss is arranged, band turps smell, density 1.060 ~ 1.085g/cm
3Fusing point 110～1 35 ℃, 72～76 ℃ of softening temperatures (ring and ball method), boiling point about 300 ℃ (0.67kPa).30～38 ℃ of second-order transition temperatures.Specific refractory power 1.5453.216 ℃ of flash-points (opening cup).About 480 ~ 500 ℃ of burning-point.Easily oxidation in air, color and luster deepens.Can be dissolved in ethanol, ether, acetone, toluene, dithiocarbonic anhydride, ethylene dichloride, turps, sherwood oil, gasoline, oils and alkaline solution.Solubleness reduces in gasoline.Be insoluble to cold water, be slightly soluble in hot water.Rosin has premium propertiess such as increasing glutinous, emulsification, softening, moistureproof, anticorrosion, insulation, and weak point is that the crystallization tendency is big in solvent.The crystallinity of rosin, be since rosin in isomer due to some solvent Shen solubleness is different with the moisture in the rosin.Rosin moisture content＜0.15% is non-crystallizable,〉0.15% easy crystallization, 0.16% serious crystallization.CRYSTALLIZATION OF ROSIN is one of major issue that influences rosin quality, can make sizing agent floss or precipitation small-particle occur, also makes glue become opaque.The crystallinity of rosin can detect with laxative remedy: get 10g rosin l fragment and 10ml acetone and place test tube, jam-pack, dissolve, leave standstill, if separate out the then easy crystallization of this rosin at the 15min intercrystalline; As behind 2h, just separating out, show that this rosin is difficult for crystallization, can relievedly use.
The quality of rosin is decided according to color, acid number, softening temperature, transparency etc.General color is more shallow, and quality better.Sylvic acid content the more, acid number is bigger, softening temperature is higher.
The stickiness of rosin is excellent, and especially pressure-sensitive, fast stickiness, low temperature stickiness are fine, but force of cohesion is relatively poor.Because rosin contains two keys and carboxyl, has stronger reactivity, thus to light, heat, oxygen than destabilization, show that ageing resistance is bad, weathering resistance is not good, be easy to generate efflorescence and metachromatism, the superfine dust of rosin and AIR MIXTURES have explosion hazard.Rosin is divided into totally 6 grades of spies,, two, three, four, five.
Summary of the invention
The purpose of this invention is to provide a kind of method for the preparation of light odorlessness rosin, it is darker to overcome general rosin color, easily oxidation by air variable color, and the shortcoming with sharp aroma.
In order to achieve the above object, the invention provides a kind of preparation method of rosin, wherein, this method comprises:
Step 1 is dissolved in optimum solvent with rosin, removes by filter insoluble impurities; Stir down, again to the non-benign solvent that wherein adds resinous acid, normal temperature leaves standstill to be handled 1 ~ 10 hour, filtered collecting precipitation; Filtrate adds thermal distillation, reclaims described optimum solvent, behind the surplus solution cool to room temperature, filters collecting precipitation again; Filtrate is merged, add thermal distillation and reclaim the non-benign solvent; Step 2 has been deposited in N with gained
2Or CO
2Add thermal isomerization processing 1 ~ 3 hour under protection, 150 ~ 180 ℃ of conditions, cooling obtains rough rosin; Step 3 is packed the rough rosin of gained in the encloses container into, is warmed up to 250 ~ 265 ℃, collects cut, and in addition condensation is deposited; Temperature is raised to 270 ~ 280 ℃ again; make rosin be converted into gaseous state by liquid state; be cooled to 230 ~ 250 ℃ then, make rosin be converted into liquid state by gaseous state, and it is transferred in the reaction vessel; add the rosin discoloring agent; under agitation be warmed up to 270 ℃, slowly be cooled to 180 ~ 220 ℃ again, add the rosin stablizer; be cooled to 90 ~ 120 ℃ at last, blowing packing or by the tablets press granulation.
The preparation method of above-mentioned rosin, wherein, described optimum solvent is methylene dichloride; The mass volume ratio of described rosin and methylene dichloride is 1:3 ~ 1:6.
The preparation method of above-mentioned rosin, wherein, described non-benign solvent is acetonitrile; The mass volume ratio of described rosin and acetonitrile is 1:3 ~ 1:6.
The preparation method of above-mentioned rosin, wherein, described rosin discoloring agent accounts for 0.05 ~ 0.15% of described rosin by mass percentage.
The preparation method of above-mentioned rosin, wherein, described rosin stablizer accounts for 0.05 ~ 0.15% of described rosin by mass percentage.
The preparation method of rosin provided by the invention has the following advantages:
Production technique is simple, does not need the special technique operation, less investment, and cost is low, and energy consumption is few.
Rosin with present method is produced has no irritating odor, and outward appearance is clear, colorless substantially, steady quality.
Embodiment
Below the specific embodiment of the present invention is further described.
The preparation method of rosin provided by the invention comprises:
Step 1 is dissolved in optimum solvent with rosin, removes by filter insoluble impurities; Stir down, again to the non-benign solvent that wherein adds resinous acid, normal temperature leaves standstill to be handled 1 ~ 10 hour, filtered collecting precipitation; Filtrate adds thermal distillation, reclaims optimum solvent, behind the surplus solution cool to room temperature, filters collecting precipitation again; Filtrate is merged, add thermal distillation and reclaim the non-benign solvent; Step 2 has been deposited in N with gained
2Or CO
2Add thermal isomerization processing 1 ~ 3 hour under protection, 150 ~ 180 ℃ of conditions, cooling obtains rough rosin; Step 3 is packed the rough rosin of gained in the encloses container into, is warmed up to 250 ~ 265 ℃, collects cut, and in addition condensation is deposited; Temperature is raised to 270 ~ 280 ℃ again; make rosin be converted into gaseous state by liquid state; be cooled to 230 ~ 250 ℃ then, make rosin be converted into liquid state by gaseous state, and it is transferred in the reaction vessel; add the rosin discoloring agent; under agitation be warmed up to 270 ℃, slowly be cooled to 180 ~ 220 ℃ again, add the rosin stablizer; be cooled to 90 ~ 120 ℃ at last, blowing packing or by the tablets press granulation.
Wherein, optimum solvent is methylene dichloride, and the mass volume ratio of rosin and methylene dichloride is 1:3 ~ 1:6.The non-benign solvent is acetonitrile, and the mass volume ratio of rosin and acetonitrile is 1:3 ~ 1:6.The rosin discoloring agent accounts for 0.05 ~ 0.15% of rosin by mass percentage.The rosin stablizer accounts for 0.05 ~ 0.15% of rosin by mass percentage.
The proportioning of embodiment 1 ~ 3 sees the following form.
Table 1: solvent and additive formula.
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| The mass volume ratio of rosin and methylene dichloride | 1:3 | 1:4 | 1:6 |
| The mass volume ratio of rosin and acetonitrile | 1:3 | 1:5 | 1:6 |
| The rosin discoloring agent accounts for the mass percent of rosin | 0.05% | 0.1% | 0.15% |
| The mass percent of rosin stabilizer comprises rosin | 0.05% | 0.1% | 0.15% |
By above arbitrary proportioning, with the optimum solvent of the lower boiling of rosin, it is methylene dichloride, dissolving rosin, after removing by filter impurity such as insoluble wood chip, bark, fully wash with oxalic acid aqueous solution at normal temperatures, consumption of oxalic acid is 0.05 ~ 1% of rosin quality, the iron ion that removes water-soluble impurity and be combined with resinous acid divides the phase of anhydrating.Organic phase under agitation adds the non-benign solvent of resinous acid, i.e. acetonitrile is separated out the resinous acid precipitation and is the discrete particles state, leaves standstill 1 ~ 10 hour, resinous acid is fully precipitated separate out, filtered and recycled resinous acid precipitation.
Selected optimum solvent is different with the non-benign solvent boiling point, is respectively 39.8 ℃ and 81. 6 ℃, all is lower than 100 ℃, can adopt common distillation or rectificating method separated and collected, and filtrate is added thermal rectification, collects 70 ℃ of front-end volatiles, obtains lower boiling optimum solvent.Be cooled to after the room temperature again filtration under diminished pressure and collect the resinous acid precipitation of separating out for the second time, with non-good part solvent wash twice, filtrate merges, and reheat is warming up to 70 ~ 90 ℃, evaporation recovery non-benign solvent.At last; resinous acid is deposited in N2 or CO2 protection normal pressure heating down (standing hot gasization, condensation collection recovery at the remaining non-benign solvent of heat-processed); resinous acid is deposited under 150 ~ 180 ℃ the temperature carried out isomerization 1 ~ 3 hour, obtain being difficult for the rough rosin of crystallization.
The rough rosin of gained is packed into and is warmed up to 250 ~ 265 ℃ in the still kettle, collects contained heavy oil or thick aromatic hydrocarbons in the rosin, and condensation stores, and keeps this process 1 hour, and peculiar smell impurity is fully evaporated totally, the smell of removal rosin.
The temperature of still kettle is raised to 270 ~ 280 ℃; rosin is converted into gaseous state by liquid state in still kettle; be cooled to 230 ~ 250 ℃ again, rosin is converted into liquid state by gaseous state, flows in the reactor; in reactor, add the rosin discoloring agent; under agitation be warmed up to 270 ℃, slowly be cooled to 180 ~ 220 ℃ again, add the rosin stablizer; be cooled to 90 ~ 120 ℃ at last, blowing packing or by the tablets press granulation.
In above still-process, the oxidation coloring matter in the rosin is removed the overwhelming majority, last surplus is eliminated with discoloring agent, is close to water white transparency so with the naked eye see products therefrom.Rosin is under vacuum gasifying state and 270 ~ 280 ℃ of high temperature, and the conjugated double bond in the molecular structure can disproportionation reaction take place and change into nilox resin, and conjugated double bond is most of to be destroyed and become stable, can be by airborne dioxygen oxidation and variable color.The distillation in early stage, most heavy oil and thick aromatic hydrocarbons are removed in the rosin, so smell also has been removed.
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (5)
1. the preparation method of a rosin is characterized in that, this method comprises:
Step 1 is dissolved in optimum solvent with rosin, removes by filter insoluble impurities; Stir down, again to the non-benign solvent that wherein adds resinous acid, normal temperature leaves standstill to be handled 1 ~ 10 hour, filtered collecting precipitation; Filtrate adds thermal distillation, reclaims described optimum solvent, behind the surplus solution cool to room temperature, filters collecting precipitation again; Filtrate is merged, add thermal distillation and reclaim the non-benign solvent;
Step 2 has been deposited in N with gained
2Or CO
2Add thermal isomerization processing 1 ~ 3 hour under protection, 150 ~ 180 ℃ of conditions, cooling obtains rough rosin;
Step 3 is packed the rough rosin of gained in the encloses container into, is warmed up to 250 ~ 265 ℃, collects cut, and in addition condensation is deposited; Temperature is raised to 270 ~ 280 ℃ again; make rosin be converted into gaseous state by liquid state; be cooled to 230 ~ 250 ℃ then, make rosin be converted into liquid state by gaseous state, and it is transferred in the reaction vessel; add the rosin discoloring agent; under agitation be warmed up to 270 ℃, slowly be cooled to 180 ~ 220 ℃ again, add the rosin stablizer; be cooled to 90 ~ 120 ℃ at last, blowing packing or by the tablets press granulation.
2. the preparation method of rosin as claimed in claim 1 is characterized in that, described optimum solvent is methylene dichloride; The mass volume ratio of described rosin and methylene dichloride is 1:3 ~ 1:6.
3. the preparation method of rosin as claimed in claim 1 is characterized in that, described non-benign solvent is acetonitrile; The mass volume ratio of described rosin and acetonitrile is 1:3 ~ 1:6.
4. the preparation method of rosin as claimed in claim 1 is characterized in that, described rosin discoloring agent accounts for 0.05 ~ 0.15% of described rosin by mass percentage.
5. the preparation method of rosin as claimed in claim 1 is characterized in that, described rosin stablizer accounts for 0.05 ~ 0.15% of described rosin by mass percentage.
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| CN2013101640960A CN103232816A (en) | 2013-05-07 | 2013-05-07 | Preparation method of rosin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106890473A (en) * | 2017-04-26 | 2017-06-27 | 贵州林亚达林化科技有限责任公司 | Distilling apparatus and the method using the device work softening agent |
| CN106916535A (en) * | 2017-04-28 | 2017-07-04 | 南宁市青秀区嘉利林化有限公司 | A kind of method that rosin vacuum distillation fractionates out middle oil |
| CN107011801A (en) * | 2017-04-28 | 2017-08-04 | 南宁市青秀区嘉利林化有限公司 | A kind of method that rosin vacuum distillation fractionates out heavy oil |
| CN107057579A (en) * | 2017-04-28 | 2017-08-18 | 南宁市青秀区嘉利林化有限公司 | A kind of rosin vacuum distillation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730584A (en) * | 2005-08-10 | 2006-02-08 | 张昌荣 | Light and ordorless colophony and its production method |
| CN101649160A (en) * | 2009-09-11 | 2010-02-17 | 广西民族大学 | Method for producing refined light-color rosin by using turpentine as raw material |
| CN101665660A (en) * | 2009-09-27 | 2010-03-10 | 广西民族大学 | Method of refining and processing rosin |
-
2013
- 2013-05-07 CN CN2013101640960A patent/CN103232816A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730584A (en) * | 2005-08-10 | 2006-02-08 | 张昌荣 | Light and ordorless colophony and its production method |
| CN101649160A (en) * | 2009-09-11 | 2010-02-17 | 广西民族大学 | Method for producing refined light-color rosin by using turpentine as raw material |
| CN101665660A (en) * | 2009-09-27 | 2010-03-10 | 广西民族大学 | Method of refining and processing rosin |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106890473A (en) * | 2017-04-26 | 2017-06-27 | 贵州林亚达林化科技有限责任公司 | Distilling apparatus and the method using the device work softening agent |
| CN106916535A (en) * | 2017-04-28 | 2017-07-04 | 南宁市青秀区嘉利林化有限公司 | A kind of method that rosin vacuum distillation fractionates out middle oil |
| CN107011801A (en) * | 2017-04-28 | 2017-08-04 | 南宁市青秀区嘉利林化有限公司 | A kind of method that rosin vacuum distillation fractionates out heavy oil |
| CN107057579A (en) * | 2017-04-28 | 2017-08-18 | 南宁市青秀区嘉利林化有限公司 | A kind of rosin vacuum distillation method |
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Application publication date: 20130807 |