CN104151467A - Preparation method of terpene resin - Google Patents
Preparation method of terpene resin Download PDFInfo
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- CN104151467A CN104151467A CN201410414126.3A CN201410414126A CN104151467A CN 104151467 A CN104151467 A CN 104151467A CN 201410414126 A CN201410414126 A CN 201410414126A CN 104151467 A CN104151467 A CN 104151467A
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- carene
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Abstract
The invention discloses a preparation method of terpene resin. The preparation method comprises the following steps: orderly adding 3-carene and a strong base solution into a reactor, heating under stirring, maintaining the temperature, washing with water, removing the water so as to obtain a solution (I); dropwise adding the solution (I) into a reactor containing toluene and anhydrous aluminum trichloride to carry out polymerization reactions; adding hot water, controlling the solution temperature, stirring, allowing the system to stand still so as to carry out layering, collecting the oil layer solution, distilling, and performing vacuum steam stripping so as to obtain the terpene resin. The preparation method utilizes 3-carene to prepare terpene resin, enlarges the application range of 3-carene, and provides a low-cost technology to prepare terpene resin.
Description
Technical field
The present invention relates to chemical industry resin deep process technology field, especially a kind of preparation method of terpine resin.
Background technology
Terpine resin is the solid thermoplastics of yellow transparent, fragility, has the performances such as nontoxic, odorless, radiation hardness, Yao crystallization, more stable to oxygen, heat, light, various synthetics are had to good intermiscibility, acid and alkali-resistance, tackifying is strong, electrical insulating property is strong, water insoluble and ethanol.Be widely used in the fields such as sizing agent, coating, rubber, leather and wrapping material.
At present, the preparation method of terpine resin be take firpene as raw material, under Ke Shi catalyst action not, through cationoid polymerisation, make, wherein, preparing terpine resin firpene used is to extract from turps, and the step that still extracts firpene from turps is comparatively complicated, cause firpene expensive raw material price, finally increased the production cost of terpine resin.
Summary of the invention
The present invention be take 3-carene and is prepared terpine resin as raw material, and object is to solve the problem that terpine resin production cost is high.
In order to address the above problem, the technical solution used in the present invention is:
A preparation method for terpine resin, is characterized in that comprising the following steps:
A, 3-carene and strong base solution are added in reaction vessel successively, heat while stirring, treat that temperature is increased to 100 ℃～160 ℃, be incubated 2 hours～8 hours, be washed to solution and be neutral, remove moisture, obtain solution I;
B, in the reaction vessel that contains toluene and aluminum trichloride (anhydrous), drip described solution I, polyreaction 5 hours～7 hours;
C, in step B gained solution, add hot water, controlling solution temperature is 60 ℃～80 ℃, stirs 0.5 hour～1 hour, and stratification, collects oil reservoir solution, and distillation vacuumizes steam and sprays and carry, and obtains terpine resin.
In technique scheme, scheme can also be more specifically: described strong base solution is the materials such as sodium hydroxide, potassium hydroxide or potassium tert.-butoxide, and the concentration of described strong base solution is 5% ~ 35%, and the mol ratio of described 3-carene and strong base solution is 1:0.5～2.0.
Further, the temperature while dripping described solution I is-5 ℃～25 ℃, and the mass ratio of described solution I and toluene is 1:1～1.2, and the quality of described aluminum trichloride (anhydrous) is 5%～8% of described toluene total mass;
Further, described distillation temperature is 220 ℃～240 ℃.
3-carene, chemical name is 3,7,7-trimethylammonium dicyclo (4. 1. 0)-3-heptene, molecular formula C
10h
163-carene is monoterpene component important in natural essential oil, there is strong pine fragrance, 3-carene is the occurring in nature chiral source materials that contain triatomic ring few in number, mainly be present in various turps, be rich in especially in India's longleaf pine turps and Scots pine turps, can be applicable to multiple eating perfume formulation, medicine, agricultural chemicals and makeup, also can be used as agricultural chemicals and medical synthetic intermediate, is softening agent, without one of irreplaceable raw material in many valuable chemical such as infectious solvent.The 3-carene of still not take is at present prepared the report of terpine resin as raw material.
Owing to having adopted technique scheme, the present invention compared with prior art has following beneficial effect:
1, first the present invention is translated into comparatively active 2-carene to adding strong base solution in 3-carene, then 2-carene synthesizes terpine resin by polyreaction, the present invention has not only widened the range of application of 3-carene, and a kind of preparation method of brand-new terpine resin is provided.
2,3-carene price is lower, take that it prepares terpine resin as raw material, has reduced production cost.
3, this terpine resin color and luster is more shallow, and softening temperature is higher, and has good clinging power, oxidation-resistance and thermostability.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
The sodium hydroxide solution that is 5% by 100 grams of 3-carenes and 14.7 grams of concentration adds in reaction vessel, heat while stirring, treat that temperature is increased to 160 ℃, be incubated 2 hours, be washed to solution and be neutral, remove moisture, obtain solution I, under-5 ℃ of conditions, in the reaction vessel that contains 97 grams of toluene and 4.85 grams of aluminum trichloride (anhydrous)s, drip solution I, polyreaction 6 hours, after having reacted, add hot water, controlling solution temperature is 80 ℃, stir 0.5 hour, stratification, collect oil reservoir solution, under 220 ℃ of conditions, distillation, vacuumizing steam spray carries, obtain terpine resin.
Embodiment 2
The potassium tert.-butoxide solution that is 35% by 1 kilogram of 3-carene and 1.65 kilograms of concentration adds in reaction vessel, heat while stirring, treat that temperature is increased to 100 ℃, be incubated 8 hours, be washed to solution and be neutral, remove moisture, obtain solution I, under 10 ℃ of conditions, in the reaction vessel that contains 2.2 kilograms of toluene and 143 grams of aluminum trichloride (anhydrous)s, drip solution I, polyreaction 5 hours, after having reacted, add hot water, controlling solution temperature is 70 ℃, stir 0.75 hour, stratification, collect oil reservoir solution, under 240 ℃ of conditions, distillation, vacuumizing steam spray carries, obtain terpine resin.
Embodiment 3
The potassium hydroxide solution that is 20% by 10 kilograms of 3-carenes and 4.12 kilograms of concentration adds in reaction vessel, heat while stirring, treat that temperature is increased to 130 ℃, be incubated 5 hours, be washed to solution and be neutral, remove moisture, obtain solution I, under 25 ℃ of conditions, in the reaction vessel that contains 16.2 kilograms of toluene and 1.3 kilograms of aluminum trichloride (anhydrous)s, drip solution I, polyreaction 7 hours, after having reacted, add hot water, controlling solution temperature is 60 ℃, stir 1 hour, stratification, collect oil reservoir solution, under 230 ℃ of conditions, distillation, vacuumizing steam spray carries, obtain terpine resin.
Claims (3)
1. a preparation method for terpine resin, is characterized in that comprising the following steps:
A, 3-carene and strong base solution are added in reaction vessel successively, heat while stirring, treat that temperature is increased to 100 ℃～160 ℃, be incubated 2 hours～8 hours, be washed to solution and be neutral, remove moisture, obtain solution I;
B, in the reaction vessel that contains toluene and aluminum trichloride (anhydrous), drip described solution I, polyreaction 5 hours～7 hours;
C, in step B gained solution, add hot water, controlling solution temperature is 60 ℃～80 ℃, stirs 0.5 hour～1 hour, and stratification, collects oil reservoir solution, and distillation vacuumizes steam and sprays and carry, and obtains terpine resin.
2. the preparation method of terpine resin according to claim 1, it is characterized in that: described strong base solution is the materials such as sodium hydroxide, potassium hydroxide or potassium tert.-butoxide, the concentration of described strong base solution is 5% ~ 35%, and the mol ratio of described 3-carene and strong base solution is 1:0.5～2.0.
3. the preparation method of terpine resin according to claim 1, it is characterized in that: the temperature while dripping described solution I is-5 ℃～25 ℃, the mass ratio of described solution I and toluene is 1:1～1.2, and the quality of described aluminum trichloride (anhydrous) is 5%～8% of described toluene total mass;
The preparation method of terpine resin according to claim 1, is characterized in that: described distillation temperature is 220 ℃～240 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410414126.3A CN104151467A (en) | 2014-08-21 | 2014-08-21 | Preparation method of terpene resin |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410414126.3A CN104151467A (en) | 2014-08-21 | 2014-08-21 | Preparation method of terpene resin |
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| CN104151467A true CN104151467A (en) | 2014-11-19 |
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| CN201410414126.3A Pending CN104151467A (en) | 2014-08-21 | 2014-08-21 | Preparation method of terpene resin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111454399A (en) * | 2020-04-30 | 2020-07-28 | 厦门中坤化学有限公司 | Light-colored high-softening-point modified carene resin and preparation method thereof |
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| CN1631916A (en) * | 2004-11-21 | 2005-06-29 | 蓝运泉 | Production method of terpene resin |
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| CN101891862A (en) * | 2010-08-18 | 2010-11-24 | 赣州泰普化学有限公司 | Modified terpene resin and preparation method thereof |
| CN102382220A (en) * | 2011-08-30 | 2012-03-21 | 广东华林化工有限公司 | Ultralight-colored polyterprene resin production process |
| CN102964495A (en) * | 2012-11-15 | 2013-03-13 | 梧州市松桦化学品有限公司 | Synthetic method of terpene resin |
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- 2014-08-21 CN CN201410414126.3A patent/CN104151467A/en active Pending
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| CN101505959A (en) * | 2006-07-17 | 2009-08-12 | 阿利桑那化学公司 | Styrenated terpene resin as well as methods of making and using the same |
| CN101891862A (en) * | 2010-08-18 | 2010-11-24 | 赣州泰普化学有限公司 | Modified terpene resin and preparation method thereof |
| CN102382220A (en) * | 2011-08-30 | 2012-03-21 | 广东华林化工有限公司 | Ultralight-colored polyterprene resin production process |
| CN102964495A (en) * | 2012-11-15 | 2013-03-13 | 梧州市松桦化学品有限公司 | Synthetic method of terpene resin |
| CN103435195A (en) * | 2013-08-21 | 2013-12-11 | 江西麻山化工有限公司 | Method for treating acid and salty organic wastewater |
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| CN111454399A (en) * | 2020-04-30 | 2020-07-28 | 厦门中坤化学有限公司 | Light-colored high-softening-point modified carene resin and preparation method thereof |
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