CN104877076A - Preparation method of colorless terpene resin - Google Patents
Preparation method of colorless terpene resin Download PDFInfo
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- CN104877076A CN104877076A CN201510255135.7A CN201510255135A CN104877076A CN 104877076 A CN104877076 A CN 104877076A CN 201510255135 A CN201510255135 A CN 201510255135A CN 104877076 A CN104877076 A CN 104877076A
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Abstract
The invention discloses a preparation method of a colorless terpene resin, which comprises the following steps: respectively adding aluminum trichloride and a solvent into a reaction kettle, adding acrylic acid, stirring uniformly, standing, slowly, uniformly and dropwisely adding the raw material into the reaction kettle, stirring, and reacting while controlling the temperature in the reaction kettle; filtering to recover the aluminum trichloride, and distilling to recover the solvent and unreacted raw material; and adding a hydrogenation catalyst, introducing hydrogen, reacting while controlling the temperature and pressure of the reaction kettle, filtering and distilling to obtain the colorless terpene resin. The terpene resin is prepared by carrying out hydrogenation reaction on the raw material pinene by using the aluminum trichloride as the catalyst, the toluene, xylene or cyclohexane as the solvent and the acrylic acid as the modifier. The obtained product has the advantages of light color, obviously higher softening point and obviously higher water resistance, and can be widely used in the industries of plastics, paints, adhesives and the like.
Description
Technical field
The present invention relates to chemical industry resin technology field, especially a kind of preparation method of colorless terpene resin.
Background technology
Terpine resin is the product of turps deep processing, there is look shallow, low smell, high rigidity, high adhesive force, oxidation-resistance, Heat stability is good, consistency and the advantage such as solvability is good, SIS system of special EVA system, there is in the thermosols such as SBS system excellent consistency and weathering resistance and Efficient Adhesive Promotion, its product is widely used in tackiness agent, solid, double sticky tape, solvent-borne type glue, bookbinding version, look fills, adhesive plaster, alkene adhesive plaster, kraft paper stuck glue cloth, tapes labels, carpenter's glue, pressure sensitive adhesive, thermosol, seal gum, paint and the aspect such as ink and other polymkeric substance modification agent.
The existing production technique of terpine resin is: first carry out rectifying to turps and remove the raffinate after rectifying, solvent toluene and catalyzer is added again in the turps after rectifying, after turps and solvent toluene react, add hot water carry out water wash procedures, again carry out distillation after the refuse washed away by catalyzer and produce in reaction process of draining and obtain liquid resin, terpine resin has just been obtained after the toluene simultaneously included liquid resin reclaims, adopting this mode, to obtain the product color that terpine resin produces dark, limit the range of application of terpine resin product.
Summary of the invention
The object of this invention is to provide a kind of preparation method of colorless terpene resin, the preparation method of this colorless terpene resin can solve the darker problem of existing terpine resin product colour.
In order to solve the problem, the technical solution used in the present invention is:
The preparation method of colorless terpene resin of the present invention take firpene as raw material, taking aluminum chloride as catalyzer, with toluene, dimethylbenzene or hexanaphthene for solvent, take vinylformic acid as modified material, then through the terpine resin that hydrogenation reaction is prepared from, specifically comprise the following steps:
A, aluminum chloride and solvent to be added in reactor respectively, then add vinylformic acid, stir, leave standstill 10 minutes ~ 20 minutes, finally raw material is slowly evenly added dropwise in reactor, stir, controlling reactor temperature is 5 DEG C ~ 20 DEG C, reacts 2 hours ~ 5 hours;
B, filtered and recycled aluminum chloride, distillating recovering solvent and unreacted raw material;
C, add hydrogenation catalyst, pass into hydrogen, control temperature of reaction kettle and pressure, reaction, filter, distillation obtains colorless terpene resin.
In technique scheme, scheme can also be more specifically: step A Raw, catalyzer, and solvent and acrylic acid mass ratio are 1:0.1 ~ 0.3:2 ~ 5:0.02 ~ 0.2.
Further, the time for adding of step A Raw is 1 hour ~ 2 hours.
Further, in step C, hydrogenation catalyst is the sulfide of nickel-molybdenum.
Further, step C temperature of reaction is 210 DEG C ~ 230 DEG C, and reaction pressure is 50,000 grams/cm ~ 800,000 grams/cm.
Owing to have employed technique scheme, the present invention compared with prior art has following beneficial effect:
The present invention take firpene as raw material, take aluminum chloride as catalyzer, with toluene, dimethylbenzene or hexanaphthene for solvent, take vinylformic acid as modified material, then through terpine resin that hydrogenation reaction is prepared from, products obtained therefrom color is more shallow, and the softening temperature of product and water repelling property are all significantly improved, and can be widely used in the industries such as plastics, paint, sizing agent.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
The preparation method of the present embodiment colorless terpene resin is: aluminum chloride and hexanaphthene are added respectively in reactor, then vinylformic acid is added, stir, leave standstill 10 minutes, finally slowly evenly be added dropwise in reactor by firpene, time for adding is 1.5 hours, stirs, controlling reactor temperature is 5 DEG C, reacts 5 hours; Filtered and recycled aluminum chloride, distillating recovering solvent and unreacted raw material; Add the sulfide of nickel-molybdenum, pass into hydrogen, controlling temperature of reaction kettle is 210 DEG C, and reacting kettle inner pressure is 50,000 grams/cm, and reaction is filtered, and distillation obtains colorless terpene resin.
Firpene in the present embodiment, aluminum chloride, hexanaphthene and acrylic acid mass ratio are 1:0.1:5:0.02.
Embodiment 2
The preparation method of the present embodiment colorless terpene resin is: aluminum chloride and toluene are added respectively in reactor, then vinylformic acid is added, stir, leave standstill 20 minutes, finally slowly evenly be added dropwise in reactor by firpene, time for adding is 2 hours, stirs, controlling reactor temperature is 10 DEG C, reacts 3.5 hours; Filtered and recycled aluminum chloride, distillating recovering solvent and unreacted raw material; Add the sulfide of nickel-molybdenum, pass into hydrogen, controlling temperature of reaction kettle is 220 DEG C, and reacting kettle inner pressure is 800,000 grams/cm, and reaction is filtered, and distillation obtains colorless terpene resin.
Firpene in the present embodiment, aluminum chloride, toluene and acrylic acid mass ratio are 1:0.3:2:0.1.
Embodiment 3
The preparation method of the present embodiment colorless terpene resin is: aluminum chloride and dimethylbenzene are added respectively in reactor, then vinylformic acid is added, stir, leave standstill 15 minutes, finally slowly evenly be added dropwise in reactor by firpene, time for adding is 1 hour, stirs, controlling reactor temperature is 20 DEG C, reacts 2 hours; Filtered and recycled aluminum chloride, distillating recovering solvent and unreacted raw material; Add the sulfide of nickel-molybdenum, pass into hydrogen, controlling temperature of reaction kettle is 230 DEG C, and reacting kettle inner pressure is 400,000 grams/cm, and reaction is filtered, and distillation obtains colorless terpene resin.
Firpene in the present embodiment, aluminum chloride, dimethylbenzene and acrylic acid mass ratio are 1:0.2:4:0.2.
Claims (5)
1. a preparation method for colorless terpene resin, is characterized in that with firpene being raw material, take aluminum chloride as catalyzer, with toluene, dimethylbenzene or hexanaphthene for solvent, take vinylformic acid as modified material, then through the terpine resin that hydrogenation reaction is prepared from, specifically comprise the following steps:
A, aluminum chloride and solvent to be added in reactor respectively, then add vinylformic acid, stir, leave standstill 10 minutes ~ 20 minutes, finally raw material is slowly evenly added dropwise in reactor, stir, controlling reactor temperature is 5 DEG C ~ 20 DEG C, reacts 2 hours ~ 5 hours;
B, filtered and recycled aluminum chloride, distillating recovering solvent and unreacted raw material;
C, add hydrogenation catalyst, pass into hydrogen, control temperature of reaction kettle and pressure, reaction, filter, distillation obtains colorless terpene resin.
2. the preparation method of colorless terpene resin according to claim 1, is characterized in that: step A Raw, catalyzer, and solvent and acrylic acid mass ratio are 1:0.1 ~ 0.3:2 ~ 5:0.02 ~ 0.2.
3. the preparation method of the colorless terpene resin according to claims 1 or 2, is characterized in that: the time for adding of step A Raw is 1 hour ~ 2 hours.
4. the preparation method of colorless terpene resin according to claim 1, is characterized in that: in step C, hydrogenation catalyst is the sulfide of nickel-molybdenum.
5. the preparation method of colorless terpene resin according to claim 1, is characterized in that: step C temperature of reaction is 210 DEG C ~ 230 DEG C, and reaction pressure is 50,000 grams/cm ~ 800,000 grams/cm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510255135.7A CN104877076A (en) | 2015-05-19 | 2015-05-19 | Preparation method of colorless terpene resin |
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| CN201510255135.7A CN104877076A (en) | 2015-05-19 | 2015-05-19 | Preparation method of colorless terpene resin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106008815A (en) * | 2016-06-27 | 2016-10-12 | 梧州市嘉盈树胶有限公司 | Preparation method of light-colored terpene resin |
| CN107880160A (en) * | 2017-11-20 | 2018-04-06 | 罗定市星光化工有限公司 | A kind of preparation method of colourless hydrogenated terpene resin |
| CN112341571A (en) * | 2020-11-19 | 2021-02-09 | 濮阳市新豫石油化工有限责任公司 | Hydrogenation method of terpene resin |
Citations (5)
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| SU1435580A1 (en) * | 1986-12-01 | 1988-11-07 | Белорусский Политехнический Институт | Method of producing copolymer methacrylic acid with terpenes |
| CN1709927A (en) * | 2005-07-08 | 2005-12-21 | 广西大学 | Method for preparing colorless terpene resin |
| 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 |
| CN102633920A (en) * | 2012-05-02 | 2012-08-15 | 无锡信达胶脂材料有限公司 | Production method of terpene resin |
| WO2014012937A2 (en) * | 2012-07-17 | 2014-01-23 | Hovis International B.V. | Method for the manufacture of a terpene-based polymer |
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2015
- 2015-05-19 CN CN201510255135.7A patent/CN104877076A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| SU1435580A1 (en) * | 1986-12-01 | 1988-11-07 | Белорусский Политехнический Институт | Method of producing copolymer methacrylic acid with terpenes |
| CN1709927A (en) * | 2005-07-08 | 2005-12-21 | 广西大学 | Method for preparing colorless terpene resin |
| 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 |
| CN102633920A (en) * | 2012-05-02 | 2012-08-15 | 无锡信达胶脂材料有限公司 | Production method of terpene resin |
| WO2014012937A2 (en) * | 2012-07-17 | 2014-01-23 | Hovis International B.V. | Method for the manufacture of a terpene-based polymer |
Non-Patent Citations (1)
| Title |
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| VOROBEVA, EV等: "SURFACE-ACTIVE PROPERTIES OF A COPOLYMER OF METHACRYLIC-ACID WITH ALPHA-PINENE", 《COLLOID JOURNAL OF THE RUSSIAN ACADEMY OF SCIENCES》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106008815A (en) * | 2016-06-27 | 2016-10-12 | 梧州市嘉盈树胶有限公司 | Preparation method of light-colored terpene resin |
| CN107880160A (en) * | 2017-11-20 | 2018-04-06 | 罗定市星光化工有限公司 | A kind of preparation method of colourless hydrogenated terpene resin |
| CN112341571A (en) * | 2020-11-19 | 2021-02-09 | 濮阳市新豫石油化工有限责任公司 | Hydrogenation method of terpene resin |
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Application publication date: 20150902 |