CN1304508C - Process for removing insoluble matter in solution of polycolophony methylbenzene - Google Patents
Process for removing insoluble matter in solution of polycolophony methylbenzene Download PDFInfo
- Publication number
- CN1304508C CN1304508C CNB2005101307959A CN200510130795A CN1304508C CN 1304508 C CN1304508 C CN 1304508C CN B2005101307959 A CNB2005101307959 A CN B2005101307959A CN 200510130795 A CN200510130795 A CN 200510130795A CN 1304508 C CN1304508 C CN 1304508C
- Authority
- CN
- China
- Prior art keywords
- solution
- rosin
- polymerized rosin
- solvent
- insoluble
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Developing Agents For Electrophotography (AREA)
Abstract
The present invention provides a method for removing insoluble substances in a polymerized rosin toluene solution, which belongs to the technical field of rosin processing. Insoluble alkaline substances are added into a polymerized rosin solution, and the adding quantity accounts for 0.01% to 20% of the quality of the rosin; the insoluble substances in the solution system are separated after the solution system is heated to 30 to 200DEG C and thermally insulated for 1 to 200 minutes; then, the rosin solution is recovered with solvents to release the rosin; the produced polymerized rosin is prepared into a 1:1 toluene solution having an insoluble substance content lower than 0.01%. The present invention has the advantages of simple process, rapidness, low cost and effective reduction of the insoluble substances in the polymerized rosin toluene solution.
Description
Technical field
The invention belongs to the rosiny processing technique field, a kind of method of removing insolubles in the solution of polycolophony methylbenzene particularly is provided, be applicable to the production of polymerized rosin.
Background technology
Polymerized rosin is Abietyl modified product, advantages such as lighter color, software point are high, non-crystallizable because polymerized rosin has, not oxidation, be widely used in the production of printing ink, paint, tackiness agent and synthetic resins etc., also be applied to rubber, electric, papermaking simultaneously and make multiple auxiliary agent etc.But the toluene insolubles in the polymerized rosin is ubiquity in homemade polymerized rosin, and this is a problem that can not be ignored.The existence of toluene insolubles had both influenced quality product, had also increased cost.So, remove toluene insolubles in the polymerized rosin particularly important that seems.Yet, up to the present, the domestic removal that does not still have technology preferably can realize the toluene insolubles in the polymerized rosin.
The general Production Flow Chart of polymerized rosin is: rosin is pulverized, added dissolution with solvents, add catalyzer then and carry out polyreaction, add solvent after reaction is finished and remove acid sludge, wash, distill, obtain polymerized rosin.
Summary of the invention
The objective of the invention is to, a kind of method of removing insolubles in the solution of polycolophony methylbenzene is provided, on the basis that does not influence the polymerized rosin performance, the content of the toluene insolubles in the polymerized rosin is dropped to below 0.01%.
The present invention can realize by dual mode:
1, in producing the polymerized rosin process, after washing, before the recovery solvent, to rosin solution (can be the solution of producing in the polymerized rosin process, also can be to be dissolved in the solution that solvent obtains with polymerized rosin, can also be the mixed solution of the two) add the alkaline matter that is insoluble to solvent (consumption be rosin quality 0.01%～20%) in the system, system is heated, after reacting 1～200 minute under 30～200 ℃ of conditions, separate insolubles, preferably 80～150 ℃ of temperature during insulation, soaking time preferably 2～30 minutes.Then rosin solution system process is routinely reclaimed solvent, put fragrant operation.The content of insolubles is below 0.01% when being mixed with 1: 1 toluene solution with the polymerized rosin of aforesaid method production.
The alkaline matter that is insoluble to rosin solution of the present invention is easy and the isolating solid-state or fluent meterial of rosin solution, it also can be solidliquid mixture, solid matter preferably, comparative optimization is a kind in the alkaline matter that forms of alkalimetal ion or alkaline-earth metal ions and weak acid radical ion or hydroxide ion, comprising: the oxyhydroxide of basic metal and alkaline-earth metal or carbonate.
Solvent in the polymerized rosin solution of the present invention is: in alkane or the aromatic hydrocarbon solvent 1～2 kind, in preferred gasoline, the benzene,toluene,xylene 1～2 kind.
2, polymerized rosin product and solvent are pressed polymerized rosin: the mass ratio of solvent=0.05～10 drops into reactor, add the alkaline matter that is insoluble to solvent, as the oxyhydroxide of basic metal and alkaline-earth metal or carbonate (consumption be rosin quality 0.01%～20%), heated and stirred makes the rosin dissolving, after reacting 1～200 minute under 30～200 ℃ of conditions, separate insolubles, then solvent is separated from system.The content of insolubles is below 0.01% when being mixed with 1: 1 toluene solution with the polymerized rosin of aforesaid method production.
The polymerized rosin solution that the present invention adds insoluble alkaline matter can be the solution of producing in the polymerized rosin process, also can be to be dissolved in the solution that solvent obtains with polymerized rosin, can also be the mixed solution of the two.
The invention has the advantages that technology is simple, quick, cost is low, can effectively reduce the insolubles in the solution of polycolophony methylbenzene.
Embodiment
Embodiment 1:
When producing polymerized rosin, before reclaiming solvent step, in the rosin solution system, add the anhydrous sodium carbonate that accounts for rosin quality 5%, be heated to 80 ℃ and react the insolubles in the separating liquid after 10 minutes, then clarifying rosin solution is shifted into distillation plant, proceed later recovery solvent, put steps such as perfume (or spice).The content of insolubles was below 0.01% when the polymerized rosin of gained was mixed with 1: 1 toluene solution.
Embodiment 2:
When producing polymerized rosin, before reclaiming solvent step, in the rosin solution system, add the Anhydrous potassium carbonate that accounts for rosin quality 1%, insolubles after heating and maintenance refluxed 15 minutes in the separating liquid, then clarifying rosin solution is shifted into distillation plant, proceed later recovery solvent, put steps such as perfume (or spice).The content of insolubles was below 0.01% when the polymerized rosin of gained was mixed with 1: 1 toluene solution.
Embodiment 3:
When producing polymerized rosin, before reclaiming solvent step, in the polymerized rosin solution system, add the lithium hydroxide that accounts for rosin quality 0.5%, insolubles after heating and maintenance refluxed 25 minutes in the separating liquid, then clarifying rosin solution is shifted into distillation plant, proceed later recovery solvent, put steps such as perfume (or spice).The content of insolubles was below 0.01% when the polymerized rosin of gained was mixed with 1: 1 toluene solution.
Embodiment 4:
In reactor, add polymerized rosin 100Kg, gasoline 200Kg, sodium hydroxide 5Kg, after stirring makes the rosin dissolving, reactor is heated to gasoline to come to life, keep boiling to separate insolubles in the solution after 5 minutes, clarifying rosin solution is shifted into distillation plant, carry out follow-up recovery solvent, put step such as perfume (or spice).The content of insolubles was below 0.01% when the polymerized rosin of gained was mixed with 1: 1 toluene solution.
Embodiment 5:
In reactor, add polymerized rosin 150Kg, dimethylbenzene 100Kg, potassium hydroxide 0.5Kg, after stirring makes the rosin dissolving, reactor is heated to 140 ℃, be incubated the insolubles that separates after 1 minute in the solution, clarifying rosin solution is shifted into distillation plant, carry out follow-up recovery solvent, put steps such as perfume (or spice).The content of insolubles was below 0.01% when the polymerized rosin of gained was mixed with 1: 1 toluene solution.
Embodiment 6:
In reactor, add polymerized rosin 100Kg, toluene 100Kg, calcium hydroxide 2Kg, after stirring makes the rosin dissolving, polymerized rosin solution in the reactor is heated to 110 ℃, be incubated the insolubles that separates after 15 minutes in the solution, clarifying rosin solution is shifted into distillation plant, carry out follow-up recovery solvent, put steps such as perfume (or spice).The content of insolubles was below 0.01% when the polymerized rosin of gained was mixed with 1: 1 toluene solution.
Embodiment 7:
In reactor, add polymerized rosin 150Kg, dimethylbenzene 50Kg, gasoline 100Kg, potassium hydroxide 0.5Kg, stirring is heated to 110 ℃ with reactor after making the rosin dissolving, is incubated the insolubles that separates after 200 minutes in the solution, clarifying rosin solution is shifted into distillation plant, carry out follow-up recovery solvent, put steps such as perfume (or spice).The content of insolubles was below 0.01% when the polymerized rosin of gained was mixed with 1: 1 toluene solution.
Embodiment 8:
In reactor, add polymerized rosin 150Kg, benzene 100Kg, anhydrous sodium carbonate 1.5Kg, after stirring makes the rosin dissolving, reactor is heated to 80 ℃, be incubated the insolubles that separates after 1 minute in the solution, clarifying rosin solution is shifted into distillation plant, carry out follow-up recovery solvent, put steps such as perfume (or spice).The content of insolubles was below 0.01% when the polymerized rosin of gained was mixed with 1: 1 toluene solution.
Claims (8)
1, a kind of method of removing insolubles in the solution of polycolophony methylbenzene, the Production Flow Chart of polymerized rosin is: rosin is pulverized, added dissolution with solvents, add catalyzer then and carry out polyreaction, add solvent after reaction is finished and remove acid sludge, wash again, distill, obtain polymerized rosin; It is characterized in that: in polymerized rosin solution, add insoluble alkaline matter, add-on is 0.01%～20% of a rosin quality, solution system is heated to 30～200 ℃ and be incubated the insoluble substance that separates after 1～200 minute wherein, then polymerized rosin solution is carried out solvent recuperation, puts perfume (or spice), the polymerized rosin of producing is mixed with 1: 1 toluene solution, and the content of insolubles is below 0.01%.
2, according to the method for claim 1, it is characterized in that: the polymerized rosin solution of processing is the solution in the production polymerized rosin process, or is dissolved in the solution that solvent obtains with polymerized rosin, or the mixed solution of the two.
3, method according to claim 1 is characterized in that: after adding alkaline matter, polymerized rosin solution is heated to 80～150 ℃, is incubated 2～30 minutes.
4, according to the method for claim 1, it is characterized in that: the described alkaline matter that is insoluble to rosin solution is easy and the isolating solid-state or fluent meterial of rosin solution, or solidliquid mixture.
5, method according to claim 4 is characterized in that: the described alkaline matter that is insoluble to rosin solution is solid-state.
6, according to claim 1 or 4 described methods, it is characterized in that: the described alkaline matter that is insoluble to rosin solution is: in the alkaline matter that alkalimetal ion or alkaline-earth metal ions and weak acid radical ion or hydroxide ion form a kind.
7, method according to claim 1 is characterized in that: the solvent in the described polymerized rosin solution is: in alkane or the aromatic hydrocarbon solvent 1～2 kind.
8, according to claim 1 or 7 described methods, it is characterized in that: the solvent in the described polymerized rosin solution is: in gasoline, the benzene,toluene,xylene 1～2 kind.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101307959A CN1304508C (en) | 2005-12-30 | 2005-12-30 | Process for removing insoluble matter in solution of polycolophony methylbenzene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101307959A CN1304508C (en) | 2005-12-30 | 2005-12-30 | Process for removing insoluble matter in solution of polycolophony methylbenzene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1793260A CN1793260A (en) | 2006-06-28 |
| CN1304508C true CN1304508C (en) | 2007-03-14 |
Family
ID=36804912
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005101307959A Expired - Fee Related CN1304508C (en) | 2005-12-30 | 2005-12-30 | Process for removing insoluble matter in solution of polycolophony methylbenzene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1304508C (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1105378A (en) * | 1993-11-17 | 1995-07-19 | 中国林业科学研究院林产化学工业研究所 | High-output non-acid-residue process for preparing poly-rosin |
| CN1583923A (en) * | 2004-06-15 | 2005-02-23 | 云安县晟达松脂化工（厂）有限公司 | Producing method for high softening point polymer resin |
-
2005
- 2005-12-30 CN CNB2005101307959A patent/CN1304508C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1105378A (en) * | 1993-11-17 | 1995-07-19 | 中国林业科学研究院林产化学工业研究所 | High-output non-acid-residue process for preparing poly-rosin |
| CN1583923A (en) * | 2004-06-15 | 2005-02-23 | 云安县晟达松脂化工（厂）有限公司 | Producing method for high softening point polymer resin |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1793260A (en) | 2006-06-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101407596B (en) | Method for recycling epoxy resins and glass fibre from non-metal powder of waste printed circuit board | |
| CN101511977A (en) | Method for production of ashless coal | |
| CN1950491A (en) | Soapstock treatment | |
| CN112574783B (en) | Method for comprehensively utilizing styrene tar | |
| CN102517154A (en) | Extraction method for extracting waste white clay residual oil | |
| CN109825322B (en) | Method for extracting phenolic substances from coal tar or direct coal liquefaction oil | |
| CN1304508C (en) | Process for removing insoluble matter in solution of polycolophony methylbenzene | |
| CA2230373A1 (en) | Method for the preparation of phytosterols from tall oil pitch | |
| CN110407686B (en) | Method for separating naphthenic acid from mixed organic matter | |
| CN102838454B (en) | Purification method for tertiary butyl hydroquinone | |
| CN110813983B (en) | Method and device for recycling solid waste phenol residues produced in alkylphenol production process | |
| CN114364841A (en) | Process for extracting lignin from black liquor | |
| CN111848359B (en) | Method for separating phenolic substances in medium and low temperature coal tar | |
| CN105037082A (en) | Method for recycling paradichlorobenzene in polyphenylene sulphide production mother liquor | |
| CN113061452A (en) | Coal tar pitch quinoline insoluble extractant and extraction method thereof | |
| CN107937009A (en) | The separation method of phenolic compound in coal tar and DCL/Direct coal liquefaction product | |
| CN111378467B (en) | Method for treating cyclohexane oxidation by-product | |
| CN1810757A (en) | Process of eliminating and recovering naphthenic acid from oil product | |
| CN101255105B (en) | Method for step reclamation of naphthenic acids and phenols from diesel alkaline residue | |
| CN101613311A (en) | From neutralized rearrangement mixture, reclaim the system and method for hexanolactam | |
| CN101255106B (en) | Method for intensified neutral oil removal of diesel alkaline residue and stepwise reclamation of naphthenic acids and phenols | |
| CN111087556A (en) | Oil-water separation material and preparation method thereof | |
| CN114874836B (en) | Waste lubricating oil regeneration process and system based on alkoxy carbon cationic liquid | |
| JP2000038377A (en) | Recycling of nylon 6 products | |
| CN102634282A (en) | Novel method for softening rosin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Tianjin Hexingtan Chemical Co., Ltd. Assignor: University of Science and Technology Beijing Contract record no.: 2010120000066 Denomination of invention: Process for removing insoluble matter in solution of polycolophony methylbenzene Granted publication date: 20070314 License type: Exclusive License Open date: 20060628 Record date: 20100613 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070314 Termination date: 20141230 |
|
| EXPY | Termination of patent right or utility model |