CN101012354A - Method of preparing polymerized rosin - Google Patents
Method of preparing polymerized rosin Download PDFInfo
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- CN101012354A CN101012354A CNA2007100194204A CN200710019420A CN101012354A CN 101012354 A CN101012354 A CN 101012354A CN A2007100194204 A CNA2007100194204 A CN A2007100194204A CN 200710019420 A CN200710019420 A CN 200710019420A CN 101012354 A CN101012354 A CN 101012354A
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Abstract
The invention discloses a making method of polymeric rosin, which comprises the following steps: adding 10% rosin into 5-100% C2-6 organic acid solvent; stirring evenly; heating to dissolve rosin; adding rosin solution in the fixed bed reaction with solid acid-cationic exchange resin catalyst at 30-99 deg.c; flowing rosin solution from upwards to downwards; distilling rosin reacting liquid; obtaining rought product; distilling at 230-260 deg.c under 1-15mgHg; obtaining the polymer in the distilling flask as polymeric rosin.
Description
One, technical field
The invention belongs to a kind of preparation method of Abietyl modified product, relate in particular to a kind of preparation method of polymerized rosin.
Two, background technology
Polymerized rosin be with renewable resources rosin be raw material under the acid catalysis effect, sylvic acid obtains through cationic polymerization by after generating carbonium ion.Its main component is the rosin dimerization body.He is widely used in coating; Printing ink; Tackiness agent; Industries such as chewing gum base.US 4,536, and 333 use formic acid to do polymerisation catalysts; US 4,414, and 146 use sulfuric acid to do polymerisation catalysts; Luo Jinyue; Wu Zhongmeng (chemistry of forest product and industry; 19; 4,1999.12, the research of solid superacid as catalyst synthesized polymer rosiny) use SO
2- 4/ Fe
2O
3Solid superacid as catalyst synthesized polymer rosin, they do not remove the method for washed reaction liquid in experimentation.These processing methodes also are not applied on the industrial production.At present, main production has sulfuric acid process in the suitability for industrialized production; Zinc chloride process; Sulfuric acid-zinc chloride process.Because used sulfuric acid in producing; Strong acid such as zinc chloride, serious to equipment corrosion, air ambient is polluted.After finishing polyreaction, to be washed till neutrality to reaction solution, generate a large amount of waste water and pollute with a large amount of water.In addition, because use strong acid causes the local peroxidation to reactant, produce a large amount of acid sludges.Also used gasoline aborning; Toluene is made solvent, makes the investment of operating environment and equipment requirements strengthen.This production technique belongs to emphasis pollution control enterprise now.
Three, summary of the invention
The present invention is directed to the problems referred to above, provide a kind of the use that environment is produced the sulfuric acid that pollutes; Strong acid such as zinc chloride need not washed reaction liquid, the preparation method of environment amenable polymerized rosin.
The technology of the present invention solution is: a kind of preparation method of polymerized rosin, and the preparation method is: 10 mass parts rosin are added in the organic acid solvent of 2～6 carbon of 5～100 mass parts, stirring and evenly mixing also is heated to 30～99 ℃, and rosin is all dissolved; The last step is dissolved good rosin solution to add in the fixed-bed reactor that solid acid-cation exchange resin catalyst composition is housed, fixed-bed reactor keep 30～99 ℃ of temperature, rosin solution flows through fixed-bed reactor from top to bottom, obtains the polymerized rosin reaction solution; To go up step polymerized rosin reaction solution 100～210 ℃ of distillations, solvent will all be steamed; The thick product of polymerized rosin with after the distillation of last step distills under 230～260 ℃/1～15mm Hg condition, steams responseless rosin, stays the polymerized rosin that is in the matrass; The organic acid of 2～6 carbon is acetate, propionic acid, butyric acid, isopropylformic acid, valeric acid, isovaleric acid, trimethylacetic acid, caproic acid or 2 Ethylbutanoic acid.Zeo-karb is: D001 macropore strong acid cation exchange resin GB/T 16579-1966,001*7 storng-acid cation exchange resin GB/T 13659-1992, three layers mix bed dedicated ion exchange resin HG/T 2623-94, a 001*7 strongly acidic styrene type cation exchange resin SH/T2605.01-1997, D001 large hole strong acid styrene system cation exchange resin SH/T 2605.2-1997,002SC strongly acidic styrene type cation exchange resin SH/T2605.3-1997, or dry hydrogen resin.
The present invention obtains following technique effect: 1. used solid acid-storng-acid cation exchange resin to make the rosin polymerization reaction catalyzer, this catalyzer can use repeatedly.2. solved in the preparation process in the present production technique, because used sulfuric acid; Strong acid such as zinc chloride, the equipment heavy corrosion that causes and to the pollution of air ambient.In addition, after finishing polyreaction, do not need reaction solution to be washed till neutrality, can not produce the contaminated wastewater environment, saved water resources simultaneously, reduced production cost with a large amount of water.3. avoid using strong acid to cause local peroxidation to reactant, produced the residue contamination that a large amount of acid sludges cause.4. the fixed-bed reactor of Shi Yonging can be realized continuous reaction.Operating environment and equipment are not produced pollution, are the rosin polymerization reaction production technique of environment amenable cleaning.
Four, embodiment
Embodiment 1. gets rosin 10 mass parts and puts in 30 mass parts (below the be mass parts) acetic acid solvent, slowly is heated to 60 ℃, under agitation all dissolvings.The rosin good dissolving joins in the fixed-bed reactor that D001 macropore strong acid cation exchange resin (GB/T 16579-1966) catalyzer is housed, and these fixed-bed reactor are heating before reinforced, and keeps 60 ℃ of steady temperatures.The rosin acetic acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 120 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 240 ℃/6mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 140 ℃ of softening temperatures, acid number 150mgkoH/g, No. 7, color (iron cobalt method).
Embodiment 2. gets 10 parts of rosin and puts in 10 parts of propionic acid solvents, slowly is heated to 70 ℃, under agitation all dissolvings.The rosin good dissolving joins in the fixed-bed reactor that 001*7 storng-acid cation exchange resin (GB/T13659-1992) catalyzer is housed, and these fixed-bed reactor are heating before reinforced, and keeps 40 ℃ of steady temperatures.Rosin propionic acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 141 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 236 ℃/4mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 142 ℃ of softening temperatures, acid number 151mgkoH/g, No. 6, color (iron cobalt method).
Embodiment 3. gets 10 parts of rosin and puts in 20 parts of butyric acid solvents, slowly is heated to 50 ℃, under agitation all dissolvings.The good rosin of dissolving is joined in the fixed-bed reactor that three layers of mixed bed dedicated ion exchange resin (HG/T2623-94) catalyzer are housed, and these fixed-bed reactor are heating before reinforced, and keeps 50 ℃ of steady temperatures.Rosin butyric acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 165 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 243 ℃/6mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008 89 standard analysiss, 140 ℃ of softening temperatures, acid number 148mgkoH/g, No. 7, color (iron cobalt method).
Embodiment 4. gets 10 parts of rosin and puts in 40 parts of valeric acid solvents, slowly is heated to 30 ℃, under agitation all dissolvings.The rosin good dissolving joins in the fixed-bed reactor that 001*7 strongly acidic styrene type cation exchange resin (SH/T 2605.01-1997) catalyzer is housed, and these fixed-bed reactor are heating before reinforced, and keeps 30 ℃ of steady temperatures.Rosin valeric acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 186 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 239 ℃/5mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 145 ℃ of softening temperatures, acid number 145mgkoH/g, No. 5, color (iron cobalt method).
Embodiment 5. gets 10 parts of rosin and puts in 5 parts of isovaleric acid solvents, slowly is heated to 80 ℃, under agitation all dissolvings.The rosin good dissolving joins in the fixed-bed reactor that D001 large hole strong acid styrene system cation exchange resin (SH/T 2605.2-1997) catalyzer is housed, and these fixed-bed reactor are heating before reinforced, and keeps 80 ℃ of steady temperatures.Rosin isovaleric acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 177 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 242 ℃/5mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 140 ℃ of softening temperatures, acid number 148mgkoH/g, No. 8, color (iron cobalt method).
Embodiment 6. gets 10 parts of rosin and puts in 50 parts of isopropylformic acid solvents, slowly is heated to 40 ℃, under agitation all dissolvings.The rosin good dissolving joins in the fixed-bed reactor that 002SC strongly acidic styrene type cation exchange resin (SH/T2605.3-1997) catalyzer is housed, and these fixed-bed reactor are heating before reinforced, and keeps 30 ℃ of steady temperatures.Rosin isopropylformic acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 155 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 247 ℃/6mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 141 ℃ of softening temperatures, acid number 145mgkoH/g, No. 7, color (iron cobalt method).
Embodiment 7. gets 10 parts of rosin and puts in 60 parts of trimethylacetic acid solvents, slowly is heated to 70 ℃, under agitation all dissolvings.The rosin good dissolving joins in the fixed-bed reactor that D001 macropore strong acid cation exchange resin (GB/T 16579-1966) catalyzer is housed, and these fixed-bed reactor are heating before reinforced, and keeps 70 ℃ of steady temperatures.Rosin trimethylacetic acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 164 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 241 ℃/7mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 144 ℃ of softening temperatures, acid number 149mgkoH/g, No. 6, color (iron cobalt method).
Embodiment 8. gets 10 parts of rosin and puts in 50 parts of caproic acid solvents, slowly is heated to 40 ℃, under agitation all dissolvings.The rosin good dissolving joins in the fixed-bed reactor that dry hydrogen resin (production of Tianjin resin processing plant of Nankai University) catalyzer is housed, and these fixed-bed reactor are heating before reinforced, and keeps 30 ℃ of steady temperatures.Rosin caproic acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 206 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 247 ℃/6mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 141 ℃ of softening temperatures, acid number 145mgkoH/g, No. 7, color (iron cobalt method).
Embodiment 9. gets 10 parts of rosin and puts in 60 parts of acetic acid solvents, slowly is heated to 80 ℃, under agitation all dissolvings.The rosin good dissolving joins in the fixed-bed reactor that 002SC strongly acidic styrene type cation exchange resin (SH/T2605.3-1997) catalyzer is housed, and these fixed-bed reactor are heating before reinforced, and keeps 80 ℃ of steady temperatures.The rosin acetic acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 119 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 242 ℃/5mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 140 ℃ of softening temperatures, acid number 145mgkoH/g, No. 7, color (iron cobalt method).
Embodiment 10. gets 10 parts of rosin and puts in 80 parts of propionic acid solvents, slowly is heated to 95 ℃, under agitation all dissolvings.The rosin good dissolving joins in the fixed-bed reactor that D001 large hole strong acid styrene system cation exchange resin (SH/T 2605.2-1997) catalyzer is housed, and these fixed-bed reactor are heating before reinforced, and keeps 95 ℃ of steady temperatures.Rosin propionic acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 141 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 249 ℃/7mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 142 ℃ of softening temperatures, acid number 150mgkoH/g, No. 6, color (iron cobalt method).
Embodiment 11. gets 10 parts of rosin and puts in 90 parts of acetic acid solvents, slowly is heated to 30 ℃, under agitation all dissolvings.The rosin good dissolving joins in the fixed-bed reactor that dry hydrogen resin (production of Tianjin resin processing plant of Nankai University) catalyzer is housed, and these fixed-bed reactor are heating before reinforced, and keeps 30 ℃ of steady temperatures.The rosin acetic acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 119 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 240 ℃/5mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 141 ℃ of softening temperatures, acid number 141mgkoH/g, No. 6, color (iron cobalt method).
Embodiment 12. gets 10 parts of rosin and puts in 100 parts of acetic acid solvents, slowly is heated to 99 ℃, under agitation all dissolvings.The good rosin of dissolving is joined in the fixed-bed reactor that three layers of mixed bed dedicated ion exchange resin (HG/T2623-94) catalyzer are housed, and these fixed-bed reactor are heating before reinforced, and keeps 99 ℃ of steady temperatures.The rosin acetic acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 119 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 247 ℃/6mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 142 ℃ of softening temperatures, acid number 150mgkoH/g, No. 7, color (iron cobalt method).
Embodiment 13. gets 10 parts of rosin and puts in 100 parts of 2 Ethylbutanoic acid solvents, slowly is heated to 90 ℃, under agitation all dissolvings.The good rosin of dissolving is joined in the fixed-bed reactor that three layers of mixed bed dedicated ion exchange resin (HG/T 2623-1994) catalyzer are housed, and these fixed-bed reactor are heating before reinforced, and keeps 90 ℃ of steady temperatures.The rosin acetic acid solution flows through fixed-bed reactor from top to bottom, and promptly polyreaction is finished.Collect reaction solution.Reaction solution is added thermal distillation at 119 ℃, solvent is all steamed, reclaim stand-by.The thick product that steams behind the solvent, in 260 ℃/15mm Hg heating underpressure distillation.Steam responseless rosin, obtain polymerized rosin.
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 142 ℃ of softening temperatures, acid number 150mgKOH/g, No. 7, color (iron cobalt method).
The preparation method of 14. 1 kinds of polymerized rosines of embodiment, the preparation method is: 10 mass parts rosin are added in the organic acid solvent of 2～6 carbon of 5～100 mass parts, stirring and evenly mixing also is heated to 30～99 ℃, and rosin is all dissolved; The last step is dissolved good rosin solution to add in the fixed-bed reactor that solid acid-cation exchange resin catalyst composition is housed, fixed-bed reactor keep 30～99 ℃ of temperature, rosin solution flows through fixed-bed reactor from top to bottom, obtains the polymerized rosin reaction solution; To go up step polymerized rosin reaction solution 100～210 ℃ of distillations, solvent will all be steamed; The thick product of polymerized rosin with after the distillation of last step distills under 230～260 ℃/1～15mmHg condition, steams responseless rosin, stays the polymerized rosin that is in the matrass;
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 142 ℃ of softening temperatures, acid number 150mgKOH/g, No. 7, color (iron cobalt method).
The preparation method of 15. 1 kinds of polymerized rosines of embodiment, the preparation method is: 10 mass parts rosin are added in the organic acid solvent of 2～6 carbon of 30～70 mass parts, stirring and evenly mixing also is heated to 40～90 ℃, and rosin is all dissolved; The last step is dissolved good rosin solution to add in the fixed-bed reactor that solid acid-cation exchange resin catalyst composition is housed, fixed-bed reactor keep 40～90 ℃ of temperature, rosin solution flows through fixed-bed reactor from top to bottom, obtains the polymerized rosin reaction solution; To go up step polymerized rosin reaction solution 150～180 ℃ of distillations, solvent will all be steamed; The thick product of polymerized rosin with after the distillation of last step distills under 236～249 ℃/5～7mmHg condition, steams responseless rosin, stays the polymerized rosin that is in the matrass;
Sampling is pressed polymerized rosin ZBB72008_89 standard analysis, 142 ℃ of softening temperatures, acid number 150mgKOH/g, No. 7, color (iron cobalt method).
Claims (7)
1. the preparation method of polymerized rosin is characterized in that the preparation method is:
A. 10 mass parts rosin are added in the organic acid solvent of 2～6 carbon of 5～100 mass parts, stirring and evenly mixing also is heated to 30～99 ℃, and rosin is all dissolved;
B. the last step being dissolved good rosin solution adds in the fixed-bed reactor that solid acid-cation exchange resin catalyst composition is housed, fixed-bed reactor keep 30～99 ℃ of temperature, rosin solution flows through fixed-bed reactor from top to bottom, obtains the polymerized rosin reaction solution;
C. will go up step polymerized rosin reaction solution 100～210 ℃ of distillations, solvent will all be steamed;
D. will go up the thick product of polymerized rosin after the step distills, under 230～260 ℃/1～15mm Hg condition, distill, steam responseless rosin, stay the polymerized rosin that is in the matrass.
2. the preparation method of polymerized rosin according to claim 1, the organic acid that it is characterized in that described 2～6 carbon is acetate, propionic acid, butyric acid, isopropylformic acid, valeric acid, isovaleric acid, trimethylacetic acid, caproic acid or 2 Ethylbutanoic acid.
3. the preparation method of polymerized rosin according to claim 1 is characterized in that described Zeo-karb is: D001 macropore strong acid cation exchange resin GB/T 16579-1966,001
*7 storng-acid cation exchange resin GB/T 13659-1992, three layers mix a bed dedicated ion exchange resin HG/T 2623-94,001
*7 strongly acidic styrene type cation exchange resin SH/T2605.01-1997, D001 large hole strong acid styrene system cation exchange resin SH/T 2605.2-1997,002SC strongly acidic styrene type cation exchange resin SH/T2605.3-1997, or dry hydrogen resin.
4. the preparation method of polymerized rosin according to claim 1 is characterized in that stirring and evenly mixing also is heated to 40～90 ℃, and rosin is all dissolved in the described organic acid solvent that 10 mass parts rosin is added 2～6 carbon of 30～70 mass parts.
5. the preparation method of polymerized rosin according to claim 1, it is characterized in that the described rosin solution that dissolving is got well adds in the fixed-bed reactor that solid acid-cation exchange resin catalyst composition is housed, fixed-bed reactor keep 40～90 ℃ of temperature, rosin solution flows through fixed-bed reactor from top to bottom, obtains the polymerized rosin reaction solution.
6. the preparation method of polymerized rosin according to claim 1, it is characterized in that described with the polymerized rosin reaction solution 150～180 ℃ of distillations, solvent is all steamed, obtain the thick product of polymerized rosin.
7. the preparation method of polymerized rosin according to claim 1 is characterized in that describedly with the thick product of polymerized rosin, distills under 236～249 ℃/5～7mm Hg condition, steams responseless rosin, stays to be the polymerized rosin product in the matrass.
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| CNA2007100194204A CN101012354A (en) | 2007-01-22 | 2007-01-22 | Method of preparing polymerized rosin |
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| CNA2007100194204A CN101012354A (en) | 2007-01-22 | 2007-01-22 | Method of preparing polymerized rosin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838502A (en) * | 2010-04-16 | 2010-09-22 | 新洲(武平)林化有限公司 | Method for colophony isomerization by cation exchange resin |
| CN102344751A (en) * | 2011-06-30 | 2012-02-08 | 广西大学 | Method for simultaneously preparing terpene rosin resin and polymerized rosin from rosin as raw material |
| CN106085243A (en) * | 2016-06-27 | 2016-11-09 | 梧州市嘉盈树胶有限公司 | The preparation method of pale rosin glyceride |
| CN108727988A (en) * | 2018-06-27 | 2018-11-02 | 广西浙缘农业科技有限公司 | The production method of newtrex |
-
2007
- 2007-01-22 CN CNA2007100194204A patent/CN101012354A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838502A (en) * | 2010-04-16 | 2010-09-22 | 新洲(武平)林化有限公司 | Method for colophony isomerization by cation exchange resin |
| CN102344751A (en) * | 2011-06-30 | 2012-02-08 | 广西大学 | Method for simultaneously preparing terpene rosin resin and polymerized rosin from rosin as raw material |
| CN102344751B (en) * | 2011-06-30 | 2014-03-12 | 广西大学 | Method for simultaneously preparing terpene rosin resin and polymerized rosin from rosin as raw material |
| CN106085243A (en) * | 2016-06-27 | 2016-11-09 | 梧州市嘉盈树胶有限公司 | The preparation method of pale rosin glyceride |
| CN108727988A (en) * | 2018-06-27 | 2018-11-02 | 广西浙缘农业科技有限公司 | The production method of newtrex |
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