CN1448436A - Prep. of petroleum resin emulsion - Google Patents
Prep. of petroleum resin emulsion Download PDFInfo
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- CN1448436A CN1448436A CN 02111259 CN02111259A CN1448436A CN 1448436 A CN1448436 A CN 1448436A CN 02111259 CN02111259 CN 02111259 CN 02111259 A CN02111259 A CN 02111259A CN 1448436 A CN1448436 A CN 1448436A
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- petroleum resin
- emulsion
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- thanomin
- oleic acid
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Abstract
The petroleum resin emulsion is made of C5 petroleum resin and/or C9 petroleum resin with softening point of 60-120 deg.c. Its production process includes the following steps: mixing molten petroleum resin and oleic acid in the weight ratio of 8-12 to form solution; adding water solution of ethanolamine of concentration 5-15 wt% and in temperature 90-100 deg.c to form emulsion at 85-100 deg.c for 30-180 min with the molar ratio between oleic acid and ethanolamine being 3-4; cooling the emulsion and filtering. The production process may be realized in common reactor with stirrer, and the emulsion has average grain size below 0.5 micron, excellent stability and no bubble.
Description
Technical field
The present invention relates to the preparation method of petroleum resin emulsion, particularly the preparation method of carbon five, C 9 petroleum resin or carbon five, carbon nine copolymerized petroleum resin emulsions.
Background technology
Petroleum resin emulsion can be used for various water accacks as a kind of tackifier, in the acrylic emulsion tackiness agent, improves its adhesive property.In prior art, the preparation method of many petroleum resin emulsions has been proposed.As patent US2,8 09,948 and US3,377, proposing with the organic solvent-free in 298 is the petroleum resin emulsion preparation technology of emulsifying agent, and it carries out violent stirring with water respectively with the fused petroleum resin in the presence of nonionogenic tenside and anion surfactant, obtain stable emulsion.Patent USP4, the inventions before 486,563 pairs improve, adopting nonionogenic tenside or anion surfactant is emulsifying agent, the petroleum resin softening temperature is adjusted to 95 ℃ of left and right sides fusions after, obtain petroleum resin emulsion by high-speed stirring.Yet these existing methods weak points are that they all need to adopt specific emulsifying device, and emulsion is when preparation and use, and foam is too many.Simultaneously, the emulsion that obtains is fine and smooth inadequately, and median size has been subjected to certain restriction more than 0.5 micron as its use range of a kind of tackiness agent.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of new petroleum resin emulsion, this method can adopt common stirring tank to be prepared, and the petroleum resin emulsion median size that makes is below 0.5 micron, has satisfactory stability, substantially do not produce foam, to overcome the existing in prior technology defective.
Below be the technical scheme that the present invention solves the problems of the technologies described above:
A kind of preparation method of petroleum resin emulsion, petroleum resin are carbon five, C 9 petroleum resin or carbon five, carbon nine copolymerized petroleum resins, and its softening temperature is 60～120 ℃, and this method may further comprise the steps:
1) make both thorough mixing form solution with adding oleic acid after the petroleum resin fusion, petroleum resin and oleic weight ratio are 8～12: 1;
2) above-mentioned solution being added concentration while stirring is that 5～15wt% and temperature are that 90～100 ℃ the thanomin aqueous solution makes it emulsification, emulsifying temperature is 85～100 ℃, emulsification times is 30～180 minutes, and the add-on of the thanomin aqueous solution is to determine at 3～4: 1 with the mol ratio of oleic acid and thanomin;
3) filter after the above-mentioned emulsion cooling the petroleum resin emulsion product.
According to the different requirements of product, the described emulsion of step 3 can be regulated its solid content with 80～100 ℃ water before cooling.
In aforesaid method, described petroleum resin of step 1 and oleic weight ratio are preferably 9～11: 1, and the oleic acid consumption is too low, and emulsifying effectiveness is bad, too highly then can produce more foam; In the step 2, the concentration of described ethanolamine solutions is preferably in 7～10wt%, and the too high meeting of concentration is given fully to stir and brought difficulty, too lowly then can cause unnecessary energy expenditure.In addition, emulsifying temperature is preferably 95～99 ℃.
The present invention comes down to adopt oleic acid amine soap emulsification system to prepare petroleum resin emulsion, its key is earlier oleic acid to be mixed with the fused petroleum resin fully as solvent, and then in the aqueous solution adding petroleum resin solution with thanomin, oleic acid and thanomin react generate oleic acid amine soap emulsifying agent in, carry out emulsification.Because oleic acid good dispersion in petroleum resin, the oleic acid amine soap emulsifying agent that reaction generates just can reach good dispersion at an easy rate in emulsion, and the effect of performance emulsifying agent, forms stable emulsion.
Compared with prior art, method provided by the invention can be implemented on the common reactor that has whipping appts, and gained emulsion median size has satisfactory stability below 0.5 micron, no matter does not all produce foam substantially in preparation process and use.Solid content can reach more than 50%, reaches as high as 70%.The petroleum resin emulsion product that it makes can be used as tackifier, is used for various water accacks and water-borne coatings, in acrylic emulsion, improves its adhesive property, can also be as the sizing agent of paper.
Embodiment
Below further describe details of the present invention by some embodiment, but embodiment does not mean limitation of the invention.[embodiment 1]
With 45 parts of softening temperatures is that 95 ℃ solid m-pentadiene petro-resin is put to the reactor that has whipping appts 5L, heating while stirring, the complete fusion of resin when temperature rises to 140 ℃ continue to be stirred when being cooled to 120 ℃, adds 4.5 parts of oleic acid and is stirred and make both thorough mixing.When temperature of charge was reduced to 98 ℃ in the still, being controlled at the temperature that splashes into aequum in 45 minutes and being 98 ℃ and concentration was the 8wt% thanomin aqueous solution.The add-on of the thanomin aqueous solution is to determine control emulsifying temperature be 95～99 ℃ at 3: 1 with the mol ratio of oleic acid and thanomin, and mixing speed is 800rpm.After dripping end, continue to stir again, add about 25 parts 98 ℃ hot water simultaneously, till mixing fully, whole emulsification times was controlled at 90 minutes.At last the gained emulsion is cooled to be product after filtration below 60 ℃.The umber of material by weight.
Measure solid content, stability and the median size of product, the results are shown in Table 1.[embodiment 2]
With 45 parts of softening temperatures is that 90 ℃ solid m-pentadiene petro-resin is put to the reactor that has whipping appts 5L, heating while stirring, the complete fusion of resin when temperature rises to 140 ℃ continue to be stirred when being cooled to 120 ℃, adds 4.5 parts of oleic acid and is stirred and make both thorough mixing.When temperature of charge was reduced to 98 ℃ in the still, being controlled at the temperature that splashes into aequum in 60 minutes and being 98 ℃ and concentration was the 9wt% thanomin aqueous solution.The add-on of the thanomin aqueous solution is to determine control emulsifying temperature be 95～99 ℃ at 3.5: 1 with the mol ratio of oleic acid and thanomin, and mixing speed is 800rpm.After dripping end, continue to stir again, add 18 parts 98 ℃ hot water simultaneously, till mixing fully, whole emulsification times was controlled at 120 minutes.At last the gained emulsion is cooled to be product after filtration below 60 ℃.The umber of material by weight.
Measure solid content, stability and the median size of product, the results are shown in Table 1.[embodiment 3]
With 45 parts of softening temperatures is that 90 ℃ solid m-pentadiene petro-resin is put to the reactor that has whipping appts 5L, heating while stirring, the complete fusion of resin when temperature rises to 140 ℃ continue to be stirred when being cooled to 120 ℃, adds 4.0 parts of oleic acid and is stirred and make both thorough mixing.When temperature of charge was reduced to 98 ℃ in the still, being controlled at the temperature that splashes into aequum in 60 minutes and being 98 ℃ and concentration was the 7.5wt% thanomin aqueous solution.The add-on of the thanomin aqueous solution is to determine control emulsifying temperature be 95～99 ℃ at 3: 1 with the mol ratio of oleic acid and thanomin, and mixing speed is 1200rpm.After dripping end, continue to stir again, add 30 parts 98 ℃ hot water simultaneously, till mixing fully, whole emulsification times was controlled at 90 minutes.At last the gained emulsion is cooled to be product after filtration below 60 ℃.The umber of material by weight.
Measure solid content, stability and the median size of product, the results are shown in Table 1.[embodiment 4]
With 45 parts of softening temperatures is that 85 ℃ solid m-pentadiene petro-resin is put to the reactor that has whipping appts 5L, heating while stirring, the complete fusion of resin when temperature rises to 140 ℃ continue to be stirred when being cooled to 120 ℃, adds 4.5 parts of oleic acid and is stirred and make both thorough mixing.When temperature of charge was reduced to 98 ℃ in the still, being controlled at the temperature that splashes into aequum in half an hour and being 98 ℃ and concentration was the 8wt% thanomin aqueous solution.The add-on of the thanomin aqueous solution is to determine control emulsifying temperature be 9 5～99 ℃ at 3: 1 with the mol ratio of oleic acid and thanomin, and mixing speed is 1200rpm.After dripping end, continue to stir again, add 10 parts 98 ℃ hot water simultaneously, till mixing fully, whole emulsification times was controlled at 60 minutes.At last the gained emulsion is cooled to be product after filtration below 60 ℃.The umber of material by weight.
Measure solid content, stability and the median size of product, the results are shown in Table 1.[embodiment 5]
With 45 parts of softening temperatures is that 95 ℃ solid m-pentadiene petro-resin is put to the reactor that has whipping appts 5L, heating while stirring, the complete fusion of resin when temperature rises to 140 ℃ continue to be stirred when being cooled to 120 ℃, adds 4.5 parts of oleic acid and is stirred and make both thorough mixing.When temperature of charge was reduced to 98 ℃ in the still, being controlled at the temperature that splashes into aequum in half an hour and being 98 ℃ and concentration was the 8wt% thanomin aqueous solution.The add-on of the thanomin aqueous solution is to determine control emulsifying temperature be 95～99 ℃ at 3.3: 1 with the mol ratio of oleic acid and thanomin, and mixing speed is 800rpm.After dripping end, continue to stir again, add 25 parts 98 ℃ hot water simultaneously, till mixing fully, whole emulsification times was controlled at 45 minutes.At last the gained emulsion is cooled to be product after filtration below 60 ℃.The umber of material by weight.
Measure solid content, stability and the median size of product, the results are shown in Table 1.[embodiment 6]
With 45 parts of softening temperatures is that 105 ℃ solid dicyclopentadiene petroleum resin is put to the reactor that has whipping appts 5L, heating while stirring, the complete fusion of resin when temperature rises to 140 ℃ continue to be stirred when being cooled to 120 ℃, adds 4.5 parts of oleic acid and is stirred and make both thorough mixing.When temperature of charge was reduced to 98 ℃ in the still, being controlled at the temperature that splashes into aequum in 60 minutes and being 98 ℃ and concentration was the 8wt% thanomin aqueous solution.The add-on of the thanomin aqueous solution is to determine control emulsifying temperature be 95～99 ℃ at 3: 1 with the mol ratio of oleic acid and thanomin, and mixing speed is 1000rpm.After dripping end, continue to stir again, add 25 parts 98 ℃ hot water simultaneously, till mixing fully, whole emulsification times was controlled at 120 minutes.At last the gained emulsion is cooled to be product after filtration below 60 ℃.The umber of material by weight.
Measure solid content, stability and the median size of product, the results are shown in Table 1.[embodiment 7]
With 45 parts of softening temperatures is that 100 ℃ solid carbon 9 petroleum resin is put to the reactor that has whipping appts 5L, heating while stirring, the complete fusion of resin when temperature rises to 140 ℃ continue to be stirred when being cooled to 120 ℃, adds 4.5 parts of oleic acid and is stirred and make both thorough mixing.When temperature of charge was reduced to 98 ℃ in the still, being controlled at the temperature that splashes into aequum in a hour and being 98 ℃ and concentration was the 10wt% thanomin aqueous solution.The add-on of the thanomin aqueous solution is to determine control emulsifying temperature be 95～99 ℃ at 3: 1 with the mol ratio of oleic acid and thanomin, and mixing speed is 800rpm.After dripping end, continue to stir again, add 25 parts 98 ℃ hot water simultaneously, till mixing fully, whole emulsification times was controlled at 120 minutes.At last the gained emulsion is cooled to be product after filtration below 60 ℃.The umber of material by weight.
Measure solid content, stability and the median size of product, the results are shown in Table 1.[embodiment 8]
With 45 parts of softening temperatures is that 80 ℃ C5/C9 copolymerized petroleum resin is put to the reactor that has whipping appts 5L, heating while stirring, and the complete fusion of resin when temperature rises to 120 ℃ adds 4.5 parts of oleic acid and is stirred and make both thorough mixing.When temperature of charge was reduced to 98 ℃ in the still, being controlled at the temperature that splashes into aequum in half an hour and being 98 ℃ and concentration was the 10wt% thanomin aqueous solution.The add-on of the thanomin aqueous solution is to determine control emulsifying temperature be 95～99 ℃ at 3: 1 with the mol ratio of oleic acid and thanomin, and mixing speed is 800rpm.After dripping end, continue to stir again, add 24 parts 98 ℃ hot water simultaneously, till mixing fully, whole emulsification times was controlled at 45 minutes.At last the gained emulsion is cooled to be product after filtration below 60 ℃.The umber of material by weight.
Measure solid content, stability and the median size of product, the results are shown in Table 1.Table 1.
| Solid content (%) | Stability | Median size (μ m) | |
| Embodiment 1 | ????55 | Good | ????0.37 |
| Embodiment 2 | ????60 | Good | ????0.40 |
| Embodiment 3 | ????50 | Good | ????0.48 |
| Embodiment 4 | ????65 | Good | ????0.46 |
| Embodiment 5 | ????55 | Good | ????0.33 |
| Embodiment 6 | ????55 | Good | ????0.45 |
| Embodiment 7 | ????55 | Good | ????0.43 |
| Embodiment 8 | ????55 | Good | ????0.35 |
Annotate: 1. solid content is pressed the GB2793 standard test;
2. stability criterion is estimated no sedimentation and is layered as by leaving standstill under the room temperature 30 days;
3. particle diameter employing electron microscope is got according to method and is recorded.
Claims (5)
1, a kind of preparation method of petroleum resin emulsion, petroleum resin are carbon five, C 9 petroleum resin or carbon five, carbon nine copolymerized petroleum resins, and its softening temperature is 60～120 ℃, and this method may further comprise the steps:
1) make both thorough mixing form solution with adding oleic acid after the petroleum resin fusion, petroleum resin and oleic weight ratio are 8～12: 1;
2) above-mentioned solution being added concentration while stirring is that 5～15wt% and temperature are that 90～100 ℃ the thanomin aqueous solution makes it emulsification, emulsifying temperature is 85～100 ℃, emulsification times is 30～180 minutes, and the add-on of the thanomin aqueous solution is to determine at 3～4: 1 with the mol ratio of oleic acid and thanomin;
3) filter after the above-mentioned emulsion cooling the petroleum resin emulsion product.
2, the preparation method of petroleum resin emulsion according to claim 1 is characterized in that the described emulsion of step 3 regulates its solid content with 80～100 ℃ water before cooling.
3, the preparation method of petroleum resin emulsion according to claim 1 and 2 is characterized in that described petroleum resin of step 1 and oleic weight ratio are preferably 9～11: 1.
4, the preparation method of petroleum resin emulsion according to claim 1 and 2 is characterized in that the described thanomin concentration of aqueous solution of step 2 is 7～10wt%
5, the preparation method of petroleum resin emulsion according to claim 1 and 2 is characterized in that the described emulsifying temperature of step 2 is preferably 95～99 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021112592A CN1180021C (en) | 2002-04-04 | 2002-04-04 | Prep. of petroleum resin emulsion |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021112592A CN1180021C (en) | 2002-04-04 | 2002-04-04 | Prep. of petroleum resin emulsion |
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| CN1448436A true CN1448436A (en) | 2003-10-15 |
| CN1180021C CN1180021C (en) | 2004-12-15 |
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| CNB021112592A Expired - Lifetime CN1180021C (en) | 2002-04-04 | 2002-04-04 | Prep. of petroleum resin emulsion |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102704338A (en) * | 2012-05-08 | 2012-10-03 | 华南理工大学 | Sizing reinforcing agent and preparation process and application thereof |
| CN104845034A (en) * | 2015-05-07 | 2015-08-19 | 成都杰晟蜀邦新材料科技有限公司 | Petroleum resin emulsion and preparation method thereof |
| CN112300407A (en) * | 2020-10-27 | 2021-02-02 | 安徽同心新材料科技有限公司 | High-solid-content water-based petroleum resin emulsion and preparation method thereof |
| CN112646201A (en) * | 2020-12-18 | 2021-04-13 | 湖南林特新材料科技有限责任公司 | Preparation method of solvent-free water-based petroleum resin emulsion |
-
2002
- 2002-04-04 CN CNB021112592A patent/CN1180021C/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102704338A (en) * | 2012-05-08 | 2012-10-03 | 华南理工大学 | Sizing reinforcing agent and preparation process and application thereof |
| CN102704338B (en) * | 2012-05-08 | 2014-07-02 | 华南理工大学 | Sizing reinforcing agent and preparation process and application thereof |
| CN104845034A (en) * | 2015-05-07 | 2015-08-19 | 成都杰晟蜀邦新材料科技有限公司 | Petroleum resin emulsion and preparation method thereof |
| CN112300407A (en) * | 2020-10-27 | 2021-02-02 | 安徽同心新材料科技有限公司 | High-solid-content water-based petroleum resin emulsion and preparation method thereof |
| CN112300407B (en) * | 2020-10-27 | 2024-04-26 | 安徽同心新材料科技有限公司 | High-solid-content water-based petroleum resin emulsion and preparation method thereof |
| CN112646201A (en) * | 2020-12-18 | 2021-04-13 | 湖南林特新材料科技有限责任公司 | Preparation method of solvent-free water-based petroleum resin emulsion |
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| Publication number | Publication date |
|---|---|
| CN1180021C (en) | 2004-12-15 |
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Granted publication date: 20041215 |