CN103450395A - Preparation method of terpene resin - Google Patents
Preparation method of terpene resin Download PDFInfo
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- CN103450395A CN103450395A CN2013103796776A CN201310379677A CN103450395A CN 103450395 A CN103450395 A CN 103450395A CN 2013103796776 A CN2013103796776 A CN 2013103796776A CN 201310379677 A CN201310379677 A CN 201310379677A CN 103450395 A CN103450395 A CN 103450395A
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Abstract
The invention discloses a preparation method of terpene resin and relates to the technical field of deep processing of resin. The preparation method comprises the following preparation steps: adding toluene and anhydrous aluminum chloride used as a catalyst into a reactor, uniformly mixing, controlling the temperature in the reactor at minus 5 DEG C to minus15 DEG C, further dropwise adding raw materials for 0.5-1 hour, then performing heat preservation for 3-4 hours, stopping the reaction, washing off the catalyst with water, evaporating the solvent, recovering the toluene, and performing steam spray extraction under vacuum to get the terpene resin. According to the preparation method, the terpene resin is produced by taking byproducts, namely dipentene, terpinene and other terpene type substances during production of terpineol and camphor as main raw materials, so that the production cost is low; furthermore, the waste materials are fully utilized, the preparation process is more stable, more safe and more efficient, and an obtained finished product is lighter in color and better in quality.
Description
Technical field
The present invention relates to chemical industry resene deep process technology, especially a kind of preparation method of terpine resin.
Background technology
A kind of thermoplastic block copolymers of terpine resin, there is, the low smell of look shallow, high rigidity, high adhesive force, oxidation-resistance and Heat stability is good, the advantages such as consistency and solvability are good, particularly have good consistency and weathering resistance and Efficient Adhesive Promotion in the hot melt adhesives such as EVA system, SIS system, SBS system.Its product is widely used in the aspects such as tackiness agent, solid, double sticky tape, solvent-borne type glue, bookbinding version, look dress, adhesive plaster, alkene adhesive plaster, kraft paper stuck glue cloth, adhesive tape label, carpenter's glue, pressure sensitive adhesive, hot melt adhesive, seal gum, paint and printing ink and other polymkeric substance modification agent.
The traditional preparation method of terpine resin adopts firpene to do raw material mostly, but, along with the price of firpene constantly raises, causes the production cost of terpine resin constantly to increase, and is unfavorable for the survival and development of enterprise.So other more economical raw material of demand also becomes the main direction that enterprise reduces production costs.
Can be accompanied by the generation of other by product in the time of α-firpene artificial camphor, Terpineol 350 product, by the mode of fractionation, each component be separated.The terpenes mixture cut wherein obtained when cut point is 160 ℃～180 ℃, traditional way is this cut further do not utilized and it be used as to waste material and sell off away with cheap price, be a kind of behavior of waste in fact, also to enterprise, bring financial loss.
Summary of the invention
The invention provides the preparation method of the terpine resin that a kind of production cost is low.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: using terpenoid substance mixtures such as kautschin and terpinenes as the raw material production terpine resin.
A kind of preparation method of terpine resin comprises following preparation process:
Add in reactor and mix using toluene and as the aluminum trichloride (anhydrous) of catalyzer, described reactor temperature is-5 ℃～-15 ℃, splash into again raw material, the time for adding of raw material is 0.5～1 hour, then be incubated 3～4 hours, stopped reaction, water washes away catalyzer, steam again solvent recuperation toluene, under vacuum, the steam spray is carried, obtain this terpine resin, it is characterized in that: described raw material is the by product kautschin of firpene isomery while producing Terpineol 350 and camphor, the mixture that the terpenoid substances such as terpinene form, described terpenoid substance is to flow out the cut obtained when while producing Terpineol 350 and camphor, the reactant cut point is 160 ℃～180 ℃, while reacting in described reactor, described toluene: terpinene: the kautschin cut is 1.0～1.2:0.6～0.8:0.2～0.4 in mass ratio, the 5%-7% that described aluminum trichloride (anhydrous) is terpinene and kautschin cut total mass.
Owing to adopting technique scheme, the present invention has following beneficial effect:
1, by originally being used as, waste material is sold off the terpinene of processing, the kautschin cut uses efficiently in the present invention, replace expensive firpene in prior art to be applied in the preparation of terpine resin as main raw material it, both made terpinene, kautschin cut obtain effective utilization, increased its value, again can decrease the production cost of terpine resin, for enterprise has created more multivalence value;
2, the present invention utilizes terpinene and the collocation of kautschin cut jointly as raw material of the present invention, thereby has improved the transformation efficiency of terpine resin, and the transformation efficiency of terpine resin is reached more than 90%, and softening temperature is more than 100 ℃;
3, the catalyzer, the toluene that in the reaction, use all can be recycled its recovery.
Embodiment
Below in conjunction with specific examples, the invention will be further described:
Embodiment 1
Add in reactor and mix using toluene and as the aluminum trichloride (anhydrous) of catalyzer, reactor temperature is-5 ℃, splash into again through well-mixed terpinene and kautschin cut, time for adding is 0.5 hour, then is incubated 3 hours, stopped reaction, water washes away catalyzer, steam solvent toluene again and reclaimed, under vacuum, the steam spray is carried, and obtains this terpine resin.
Wherein, the consumption of toluene, terpinene, kautschin cut is toluene in mass ratio: terpinene: kautschin cut=1.0:0.6:0.3,5% of the total mass that the consumption of aluminum trichloride (anhydrous) is terpinene and kautschin cut.
Embodiment 2
Add in reactor and mix using toluene and as the aluminum trichloride (anhydrous) of catalyzer, reactor temperature is-10 ℃, splash into again through well-mixed terpinene and kautschin cut, time for adding is 0.8 hour, then is incubated 3.5 hours, stopped reaction, water washes away catalyzer, steam solvent toluene again and reclaimed, under vacuum, the steam spray is carried, and obtains this terpine resin.
Wherein, the consumption of toluene, terpinene, kautschin cut is toluene in mass ratio: terpinene: dihydromyrcene overhead distillate=1.1:0.7:0.2,6% of the total mass that the consumption of aluminum trichloride (anhydrous) is terpinene and dihydromyrcene overhead distillate.
Embodiment 3
Add in reactor and mix using toluene and as the aluminum trichloride (anhydrous) of catalyzer, reactor temperature is-15 ℃, splash into again through well-mixed terpinene and kautschin cut, time for adding is 1 hour, then is incubated 4 hours, stopped reaction, water washes away catalyzer, steam solvent toluene again and reclaimed, under vacuum, the steam spray is carried, and obtains this terpine resin.
Wherein, the consumption of toluene, terpinene, kautschin cut is toluene in mass ratio: terpinene: kautschin cut=1.2:0.8:0.4,7% of the total mass that the consumption of aluminum trichloride (anhydrous) is terpinene and kautschin cut.
The transformation efficiency of the terpine resin of the present invention obtained by above-described embodiment reaches more than 90%, and softening temperature is more than 100 ℃.
The detection index of the terpine resin of so producing is as following table:
According to above-mentioned data, can show that the terpine resin indices synthetic by present method is up to state standards, and give birth to material cost, greatly reduce.
Claims (1)
1. the preparation method of a terpine resin, its preparation process is as follows:
Add in reactor and mix using toluene and as the aluminum trichloride (anhydrous) of catalyzer, described reactor temperature is-5 ℃～-15 ℃, splash into again raw material, the time for adding of raw material is 0.5～1 hour, then be incubated 3～4 hours, stopped reaction, water washes away catalyzer, steam again solvent recuperation toluene, under vacuum, the steam spray is carried, obtain this terpine resin, it is characterized in that: described raw material is the by product kautschin of firpene isomery while producing Terpineol 350 and camphor, the mixture that the terpenoid substances such as terpinene form, described terpenoid substance is to flow out the cut obtained when while producing Terpineol 350 and camphor, the reactant cut point is 160 ℃～180 ℃, while reacting in described reactor, described toluene: terpinene: the kautschin cut is 1.0～1.2:0.6～0.8:0.2～0.4 in mass ratio, the 5%-7% that described aluminum trichloride (anhydrous) is terpinene and kautschin cut total mass.
Priority Applications (1)
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| CN201310379677.6A CN103450395B (en) | 2013-08-28 | 2013-08-28 | The preparation method of terpine resin |
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| CN201310379677.6A CN103450395B (en) | 2013-08-28 | 2013-08-28 | The preparation method of terpine resin |
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| CN103450395A true CN103450395A (en) | 2013-12-18 |
| CN103450395B CN103450395B (en) | 2016-01-06 |
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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 |
| CN104693329A (en) * | 2015-03-28 | 2015-06-10 | 罗定市星光化工有限公司 | Terpene resin environment-friendly production technology |
| CN104910303A (en) * | 2015-05-27 | 2015-09-16 | 梧州市嘉盈树胶有限公司 | Method for preparing terpene resin by using dipentene as raw material |
| CN104910304A (en) * | 2015-05-27 | 2015-09-16 | 梧州市嘉盈树胶有限公司 | Method for preparing terpene resin by using longifolene as raw material |
| CN111548439A (en) * | 2020-04-30 | 2020-08-18 | 广东星光脂胶科技股份有限公司 | Production process of terpene resin |
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| US4701517A (en) * | 1986-03-13 | 1987-10-20 | Hercules Incorporated | Vinyl aromatic/terpene/phenol terpolymer |
| CN102633919A (en) * | 2012-05-02 | 2012-08-15 | 中国林业科学研究院林产化学工业研究所 | Terpene resin and preparation method thereof |
| 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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2013
- 2013-08-28 CN CN201310379677.6A patent/CN103450395B/en not_active Expired - Fee Related
Patent Citations (3)
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| US4701517A (en) * | 1986-03-13 | 1987-10-20 | Hercules Incorporated | Vinyl aromatic/terpene/phenol terpolymer |
| CN102633919A (en) * | 2012-05-02 | 2012-08-15 | 中国林业科学研究院林产化学工业研究所 | Terpene resin and preparation method thereof |
| 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 |
Non-Patent Citations (1)
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| 陈清松，等: "工业双戊烯的精馏及其聚合反应影响因素", 《福建师范大学学报（自然科学版）》, vol. 19, no. 1, 31 March 2003 (2003-03-31) * |
Cited By (7)
| 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 |
| CN104211843B (en) * | 2014-08-14 | 2016-08-24 | 广西众昌树脂有限公司 | The preparation method of terpene resin |
| CN104693329A (en) * | 2015-03-28 | 2015-06-10 | 罗定市星光化工有限公司 | Terpene resin environment-friendly production technology |
| CN104693329B (en) * | 2015-03-28 | 2018-06-19 | 罗定市星光化工有限公司 | A kind of environment-friendly production process of terpene resin |
| CN104910303A (en) * | 2015-05-27 | 2015-09-16 | 梧州市嘉盈树胶有限公司 | Method for preparing terpene resin by using dipentene as raw material |
| CN104910304A (en) * | 2015-05-27 | 2015-09-16 | 梧州市嘉盈树胶有限公司 | Method for preparing terpene resin by using longifolene as raw material |
| CN111548439A (en) * | 2020-04-30 | 2020-08-18 | 广东星光脂胶科技股份有限公司 | Production process of terpene resin |
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| CN103450395B (en) | 2016-01-06 |
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