CN102633920A - Production method of terpene resin - Google Patents
Production method of terpene resin Download PDFInfo
- Publication number
- CN102633920A CN102633920A CN2012101315688A CN201210131568A CN102633920A CN 102633920 A CN102633920 A CN 102633920A CN 2012101315688 A CN2012101315688 A CN 2012101315688A CN 201210131568 A CN201210131568 A CN 201210131568A CN 102633920 A CN102633920 A CN 102633920A
- Authority
- CN
- China
- Prior art keywords
- solvent
- reaction
- terpene resin
- pinene
- production
- 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.)
- Pending
Links
Abstract
The invention relates to a production method of a terpene resin, belonging to the technical field of chemical material production. The invention is an improvement on the basis of the traditional synthesis method of a terpene resin. The production method comprises steps as follows: alpha-pinene or beta-pinene is used as the main raw material, a non-benzene solvent is used as a production solvent instead of methylbenzene or dimethylbenzene, and aluminum trichloride or an aluminum trichloride/antimony trichloride compound system is used as a catalyst; and polymerization is carried out at low temperature or normal temperature, and the product is washed with water to obtain the terpene resin. The solvent is cyclohexane and homologs thereof, and the like, which are saturated alkanes with bioinertness, and the mass ratio of the solvent to the raw material is (0.2-2.0):1; the reaction time is 1-15 hours; the catalyst accounts for 3-10% of the raw material; the reaction temperature range is -10-130 DEG C; and the reaction pressure is 0-0.3MPa (gage pressure). The production technique is simple, safe and sanitary; and the terpene resin synthesized by the method can be used in the field of gum confection bodying agents, hot-melt adhesives for food packaging, sanitary products and the like more safely.
Description
Technical field
A kind of working method of terpine resin, terpine resin are a kind of novel good tackifier, belong to the chemical materials production technical field.
Background technology
Along with people's is to the improve of food safety degree of concern, and as the terpine resin of foodstuff additive, its production process has adopted the higher toluene kind solvent of toxicity, has caused people's attention and uneasiness.Therefore to the reform of its conventional production methods, select the solvent more safer than toluene kind solvent for use, this problem is mentioned on the reform schedules naturally.The present invention adopts non-benzene kind solvent to substitute toluene or YLENE synthesizes terpine resin as producing solvent; Guaranteed that the security of product application in fields such as foodstuff additive, food product pack and human body sanitary products is improved on the one hand; Avoided using of injury and the environmental hazard of the higher material (toluene) of toxicity on the other hand, had bigger realistic meaning and social benefit the production operation personnel.The present invention simple, the safety and sanitation of method technology of synthetic terpine resin; Products obtained therefrom has excellent binding property; Heat-resisting, fast light, anti-good characteristic such as smelly, nontoxic is widely used in hot melt adhesive, printing ink, plastics, printing, health, food and food product pack industry.Because of its good chewiness becomes one of important source material of candy matrix.
Summary of the invention
The object of the invention is to seek the new working method of a kind of terpine resin, and its conventional production methods is reformed, and selects the solvent more safer than toluene kind solvent for use.
Technical scheme of the present invention: a kind of working method of terpine resin; With turps or а-firpene or beta-pinene is main raw material; Select for use alternative toluene of non-benzene kind solvent stable hydrocarbon or YLENE as producing solvent; Still adopting aluminum chloride or aluminum chloride/butter of antimony compound system is catalyzer, polymerization under low temperature or the normal temperature, and reaction product obtains qualified terpine resin product through the washing aftertreatment.
Described terpine resin raw materials for production can be the turps of China's production of generally acknowledging, or separate а-firpene, the beta-pinene of purifying and obtaining with additive method, or what mix other small amounts of olefins is master's raw material with а-firpene, beta-pinene;
It is stable hydrocarbon that said saturated hydrocarbon solvent adopts hexamethylene methane series or pentamethylene, and most typical is hexanaphthene, methylcyclohexane.Can certainly be ethylcyclohexane, dimethyl cyclohexane, or pentamethylene, methylcyclopentane.The solvent ratio of being selected for use the ratio of raw materials quality (solvent with) is 0.2～2.0 ︰ 1;
Described catalyst levels.Its consumption be raw materials quality 3%～10% between;
Described temperature of reaction can be from-10 ℃～130 ℃, and this reaction can be at synthesis under normal pressure, also can depress reaction adding, and its pressure range is at 0～0.3MPa (gauge pressure), reaction times 1～15h.
Beneficial effect of the present invention: the present invention selects for use non-benzene kind solvent to produce solvent as terpine resin through test of long duration and exploration, has reached the purpose of security and novelty.
Embodiment
Embodiment 1
In a constant temperature ice-water bath, insert the 1L four-hole boiling flask, four mouths are respectively: whisking appliance, TM, return channel and dropping mouth.In flask, drop into solvent hexanaphthene 200g, add aluminum trichloride (anhydrous) 12g, raw material adopts slash pine turps.Wherein contain а-firpene 50.53%, beta-pinene 36%～39% (remainder is all the other alkene).Turps total amount 300g, the initial stage is dropped into 150g, and all the other drip input.Above system stirs initiation reaction under 0 ℃ of condition, reaction begins temperature and rises to 20 ℃, about 10 ℃ of cooling controlled temperature, and reaction 8h, through washing aftertreatment supervisor, final product 220g, 103 ℃ of the softening temperatures of getting.
Embodiment 2
With embodiment 1 same apparatus, in flask, drop into methylcyclohexane 250g, add aluminum trichloride (anhydrous) 12g, raw material slash pine turps (composition is with embodiment 1).Turps total amount 250g, the initial stage is dropped into 150g, drips 100g, begins to stir after the end that feeds intake, and reaction is warming up to 30 ℃, reacts 8h under 20 ℃ of conditions of cooling controlled temperature, through washing aftertreatment, final product 158g, 105 ℃ of softening temperatures.
Embodiment 3
In the enamel jacketed refrigerative reaction kettle of a 50L, the oblique paddle stirrer of band mechanical seal is housed, 150 rev/mins of rotating speeds, 10L drips groove and drips in still through under meter.
Proportioning: slash pine turps (а-firpene content about 50%, beta-pinene content about 38%) 12kg
Hexanaphthene 8kg, aluminum trichloride (anhydrous) 0.6kg.
In reaction kettle, drop into whole hexanaphthenes and aluminum chloride earlier, drop into 6kg turps, start and stir; Reaction kettle water flowing cooling, controlled temperature drips remaining 6kg turps below 30 ℃ in 2h; Continue reaction 6h, the washing aftertreatment obtains terpine resin 9.5kg at last.98 ℃ of softening temperatures.
Embodiment 4
The device identical with embodiment 3, identical proportioning and condition, reaction begins to vacuumize-0.08MPa (gauge pressure).Be charged to+0.1MPa (gauge pressure), stir then and be warming up to 90 ℃, remaining 6kg turps is dripped in 2h, continue reaction 4h, temperature is controlled at 80 ℃～90 ℃.Pressure 0.1MPa ± 0.01 is washed aftertreatment at last, gets terpine resin 8.9kg, 110 ℃ of softening temperatures.
Claims (2)
1. the working method of a terpine resin is characterized in that adopting turps, or separates а-firpene, the beta-pinene of purifying and obtaining with additive method; Or what mix other small amounts of olefins is master's raw material with а-firpene, beta-pinene; Adopting hexamethylene methane series or pentamethylene is that stable hydrocarbon substitutes toluene or YLENE as producing solvent, and solvent is 0.2～2.0 ︰ 1 with the ratio of raw materials quality, and still adopting aluminum chloride or aluminum chloride/butter of antimony compound system is catalyzer; Catalyst levels is 3%～10% of a raw materials quality; Range of reaction temperature-10 ℃～130 ℃ is reflected at normal pressure or depresses reaction, its pressure gauge pressure 0-0.3mpa adding; Reaction times 1～15h, reaction product obtains qualified terpine resin product through the washing aftertreatment.
2. the working method of terpine resin according to claim 1 is characterized in that described hexamethylene methane series or pentamethylene are saturated hydrocarbon solvent, selects hexanaphthene, methylcyclohexane, ethylcyclohexane, dimethyl cyclohexane, pentamethylene or methylcyclopentane for use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101315688A CN102633920A (en) | 2012-05-02 | 2012-05-02 | Production method of terpene resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101315688A CN102633920A (en) | 2012-05-02 | 2012-05-02 | Production method of terpene resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102633920A true CN102633920A (en) | 2012-08-15 |
Family
ID=46618506
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012101315688A Pending CN102633920A (en) | 2012-05-02 | 2012-05-02 | Production method of terpene resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102633920A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211843A (en) * | 2014-08-14 | 2014-12-17 | 广西众昌树脂有限公司 | Preparation method of terpene resin |
| CN104877076A (en) * | 2015-05-19 | 2015-09-02 | 广西众昌树脂有限公司 | Preparation method of colorless terpene resin |
| CN104877075A (en) * | 2015-05-19 | 2015-09-02 | 广西众昌树脂有限公司 | Method for producing terpene resin by taking turpentine as raw material |
| CN104877074A (en) * | 2015-05-19 | 2015-09-02 | 广西众昌树脂有限公司 | Method for modifying terpene resin |
| CN104045767B (en) * | 2014-05-22 | 2016-06-01 | 宁波职业技术学院 | The preparation method of a kind of indenes modification �� pinene resin |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6201059B1 (en) * | 1999-08-19 | 2001-03-13 | The Goodyear Tire & Rubber Company | Pneumatic tire having a tread containing dicyclopentadiene/beta-pinene resin |
| JP3558172B2 (en) * | 1994-07-22 | 2004-08-25 | 荒川化学工業株式会社 | Method for producing α-pinene resin having high softening point |
| CN1709927A (en) * | 2005-07-08 | 2005-12-21 | 广西大学 | Method for preparing colorless terpene resin |
| CN101503495A (en) * | 2009-02-24 | 2009-08-12 | 宁波职业技术学院 | Preparation of alpha-pinene modified C5 hydrocarbon resin |
| US20090209720A1 (en) * | 2006-10-11 | 2009-08-20 | Yasuhara Chemical Co., Ltd. | Beta-PINENE POLYMER AND PROCESS FOR PRODUCING THE SAME |
| US20100273964A1 (en) * | 2009-04-22 | 2010-10-28 | Stewart Lewis | Heterogeneous lewis acid catalysts for cationic polymerizations |
| CN101990549A (en) * | 2008-04-10 | 2011-03-23 | 株式会社可乐丽 | Hydrogenated beta-pinene-based polymer and molded article comprising the same |
-
2012
- 2012-05-02 CN CN2012101315688A patent/CN102633920A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3558172B2 (en) * | 1994-07-22 | 2004-08-25 | 荒川化学工業株式会社 | Method for producing α-pinene resin having high softening point |
| US6201059B1 (en) * | 1999-08-19 | 2001-03-13 | The Goodyear Tire & Rubber Company | Pneumatic tire having a tread containing dicyclopentadiene/beta-pinene resin |
| CN1709927A (en) * | 2005-07-08 | 2005-12-21 | 广西大学 | Method for preparing colorless terpene resin |
| US20090209720A1 (en) * | 2006-10-11 | 2009-08-20 | Yasuhara Chemical Co., Ltd. | Beta-PINENE POLYMER AND PROCESS FOR PRODUCING THE SAME |
| CN101990549A (en) * | 2008-04-10 | 2011-03-23 | 株式会社可乐丽 | Hydrogenated beta-pinene-based polymer and molded article comprising the same |
| CN101503495A (en) * | 2009-02-24 | 2009-08-12 | 宁波职业技术学院 | Preparation of alpha-pinene modified C5 hydrocarbon resin |
| US20100273964A1 (en) * | 2009-04-22 | 2010-10-28 | Stewart Lewis | Heterogeneous lewis acid catalysts for cationic polymerizations |
Non-Patent Citations (6)
| Title |
|---|
| 《广西大学学报：自然科学版》 20090430 熊德元等 alpha-蒎烯-beta-蒎烯共聚物的热稳定性与热降解动力学 第34卷, 第2期 * |
| 《应用化学》 20060831 熊德元等 alpha-蒎烯/beta-蒎烯共聚物合成与表征 第862-865页 1-2 第23卷, 第8期 * |
| 《石油化工》 20061231 熊德元等 alpha/beta-蒎烯阳离子共混聚合工艺改进 第35卷, 第6期 * |
| 熊德元等: "α/β-蒎烯阳离子共混聚合工艺改进", 《石油化工》 * |
| 熊德元等: "α-蒎烯/β-蒎烯共聚物合成与表征", 《应用化学》 * |
| 熊德元等: "α-蒎烯-β-蒎烯共聚物的热稳定性与热降解动力学", 《广西大学学报：自然科学版》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104045767B (en) * | 2014-05-22 | 2016-06-01 | 宁波职业技术学院 | The preparation method of a kind of indenes modification �� pinene resin |
| CN104211843A (en) * | 2014-08-14 | 2014-12-17 | 广西众昌树脂有限公司 | Preparation method of terpene resin |
| CN104211843B (en) * | 2014-08-14 | 2016-08-24 | 广西众昌树脂有限公司 | The preparation method of terpene resin |
| CN104877076A (en) * | 2015-05-19 | 2015-09-02 | 广西众昌树脂有限公司 | Preparation method of colorless terpene resin |
| CN104877075A (en) * | 2015-05-19 | 2015-09-02 | 广西众昌树脂有限公司 | Method for producing terpene resin by taking turpentine as raw material |
| CN104877074A (en) * | 2015-05-19 | 2015-09-02 | 广西众昌树脂有限公司 | Method for modifying terpene resin |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102633920A (en) | Production method of terpene resin | |
| WO2012167790A3 (en) | Process for producing liquid hydrocarbon | |
| BR9810625A (en) | Propylene terpolymers and process for their production | |
| CN105439902B (en) | A kind of production technology of α cyanacrylates adhesive | |
| WO2009039948A3 (en) | Method and installation for the production of hydrocarbons | |
| RU2014102481A (en) | METHOD FOR MANUFACTURING AERIATED SHELL OF CONFECTIONERY PRODUCT | |
| RU2010114817A (en) | FUNCTIONALIZED DIENE RUBBERS WITH HIGH CONTENTS OF VINYL GROUPS | |
| MX2014002154A (en) | Oxygen scavengers. | |
| NZ594654A (en) | Base, products containing the same, preparation methods and uses thereof | |
| CN106749118A (en) | The smooth caprylate emulsifying agent of sorb | |
| CN102532379A (en) | Polymerization method for preparing rare earth isoprene rubber | |
| US2570601A (en) | Production of resins from butadiene monoxide and from mixtures of butadiene monoxide and vinyl compounds | |
| CN108689881A (en) | The synthetic method of α-n-octylcyanoacrylate | |
| CN105254872B (en) | A kind of Semi-aromatic transparent polyamide and its synthetic method containing pyridine heterocycle | |
| CN108285503B (en) | High-softening-point terpene resin and preparation method thereof | |
| CN106220853B (en) | A kind of polysulfone resin industrialized producing technology | |
| CN104256846A (en) | Tuckahoe glucose solid drink and preparation method thereof | |
| WO2009008409A1 (en) | 4-methyl-1-pentene polymer, process for production thereof, and use thereof | |
| CN110184014A (en) | A kind of high viscosity Laminating adhesive and preparation method thereof | |
| CN105330851B (en) | Long carbon chain transparent nylon and its synthetic method | |
| CN104086390A (en) | Method for preparing vanillin through sodium isoeugenol process | |
| CN101550118B (en) | Synthetic process for vitamin C sodium salts | |
| CN104178063A (en) | Pressure-sensitive adhesive | |
| CN102617951B (en) | Preparation method of polyvinyl chloride (PVC)-based material granule plasticized by non-benzene plasticizer for preparing hard or semi-hard products | |
| CN103265571A (en) | Preparation method of vinyl cyclosiloxane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120815 |