CN102911376A - Preparation method of water-based rosin resin tackifying emulsion - Google Patents
Preparation method of water-based rosin resin tackifying emulsion Download PDFInfo
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- CN102911376A CN102911376A CN2012104579014A CN201210457901A CN102911376A CN 102911376 A CN102911376 A CN 102911376A CN 2012104579014 A CN2012104579014 A CN 2012104579014A CN 201210457901 A CN201210457901 A CN 201210457901A CN 102911376 A CN102911376 A CN 102911376A
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Abstract
The invention discloses a preparation method of water-based rosin resin tackifying emulsion. The preparation method comprises the following steps of: A. adding rosin resin into an emulsification kettle, heating to the temperature higher than a softening point of the rosin resin by 5-50 DEG C, sequentially adding an emulsifier A with mass concentration of 6%-10% and an emulsifier B with mass concentration of 1%-4% while stirring, and stirring evenly; B. slow adding deionized water into the mixture obtained in the step A for emulsification, with the temperature of the deionized water close to the emulsification temperature of the rosin resin, and stirring at the speed of 80-110 RPM, and then adding deionized water at the same temperature, reducing the stirring speed to 50 RPM until fully mixing, and controlling the overall emulsification time to be 40-60 minutes; and C. cooling emulsion obtained in the step B below 60 DEG C, and filtering to obtain the product. The tackifying emulsion is good in biodegradability and very good in emulsification effect, any organic solvent is not added in production, and the obtained emulsion is exquisite, and good in stability and compatibility with polymer emulsion.
Description
Technical field
The present invention relates to technical field of chemistry, especially a kind of preparation method of water base Gum Rosin Tackified emulsion.
Background technology
Rosin is as a kind of reproducible natural resource, and is main as tackifier in tackiness agent and coating.Rosin and rosin ester are a kind of oil-soluble resins, it can only be dissolved in the organic solvent matching and could using with organic substance.Along with modern technologies development, people are to the attention of environment protection, in the industrial circles such as tackiness agent, coating, in succession develop pollution-free, nuisanceless, low-cost, and emulsion type products safe and convenient to use, i.e. " Green Product ".After the 1980s, emulsion adhesive and coating are occupied an leading position in tackiness agent and coatings industry.Rosin ester emulsion can significantly improve the performance of emulsion adhesive and coating, and can reduce the cost of coating and tackiness agent, is subject to people's generally attention, the preparation of existing many bibliographical information rosin ester emulsions.The emulsifying agent that U.S Patent5236624 report adopts negatively charged ion and nonionogenic tenside to be re-dubbed makes 40% ~ 60% emulsion particle diameter less than the rosin ester emulsion of 500nm with continuous emulsification, be used for the Tackified emulsion of water-borne pressure sensitive adhesive; China is also more active to the research of rosin ester emulsion, Wang Zhenhong etc. and thank to the sunshine philosophy and adopt the reverse emulsion process of melting to prepare the low softening point rosin ester emulsion, with the small particle size ester gum stability of emulsion of solvent hydrotropy emulsion process and the preparation of High Temperature High Pressure emulsion process above 6 months.Substantially do not have open but these research contents of Chinese scholar are not all declared relevant patent, especially emulsifying agent.
The rosin ester emulsion size directly affect emulsion stability and with the consistency of polymer emulsion, rosin ester emulsion certain stability under normal weather condition that particle diameter is large, but relatively poor at mal-condition such as high temperature, low temperature stability inferior, transportation and the use of product have been limited, simultaneously relatively poor with the consistency of polymer emulsion, be separated after causing film forming, so that film uniformity is poor, thereby cause unstable properties.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method with satisfactory stability, water base Gum Rosin Tackified emulsion that solid content is high.
In order to achieve the above object, the technical solution adopted in the present invention is: its making step of preparation method of this water base Gum Rosin Tackified emulsion is:
A, Gum Rosin is added in the emulsifying kettle, is heated to the temperature that exceeds 5 ℃ ~ 50 ℃ of its softening temperatures, under agitation add successively mass concentration and be 6% ~ 10% emulsifying agent A and 1% ~ 4% emulsifying agent B, stir;
B, slowly add the deionized water that accounts for Gum Rosin weight 10% ~ 40% through preheating in A step gains, carry out emulsification, the emulsifying temperature of deionized water temperature and Gum Rosin is close, 80 to turn ~ 110 rev/mins speed stirring; Add synthermal deionized water again, reduce mixing speed to 50 rev/min, until mix fully, whole emulsification times is 40 minutes ~ 60 minutes;
C, B step gained emulsion is cooled below 60 ℃, filter, namely get this water base Gum Rosin Tackified emulsion.
In the technique scheme, scheme can also be more specifically: in the above-mentioned B step, and 90 ℃ ~ 100 ℃ of the emulsifying temperatures of high-softening-point rosin resin, 95 ~ 100 ℃ of corresponding deionized water temperature; The emulsifying temperature of low softening point Gum Rosin is 40 ℃ ~ 70 ℃, 40 ~ 70 ℃ of corresponding deionized water temperature.
Further: among the step C, described emulsion is regulated its solid content with 80 ℃ ~ 100 ℃ deionized water before cooling.
Further: described Gum Rosin is the ester compound that makes of rosin and unit alcohol, dibasic alcohol or polyvalent alcohol generation esterification or their mixture; Unit alcohol is one or more mixtures in methyl alcohol, ethanol, propyl carbinol or the isooctyl alcohol; Dibasic alcohol is that ethylene glycol, Diethylene Glycol, glycol ether, triglycol or the polymerization degree are one or more mixtures in the polyoxyethylene glycol of 1-10; Polyvalent alcohol is one or more mixtures in glycerine, tetramethylolmethane, sorbyl alcohol or the sucrose.
Because adopt technique scheme, the present invention has following beneficial effect:
1, adopted emulsifying agent A and emulsifying agent B, biological degradability is good, does not add any organic solvent thereby preparation method's environmental protection in the production.
2, the emulsifying agent A and the emulsifying agent B that adopt, emulsifying effectiveness is fine, and the emulsion of gained is fine and smooth, and good stability is good with the consistency of polymer emulsion.
3, the present invention can implement at the common reactor with anchor formula whipping appts, no matter does not all substantially produce foam in preparation process and use procedure; Solid content can reach more than 50%, reaches as high as 65%; Its water base Gum Rosin Tackified emulsion product that makes can be used as tackifier, is used for various water accacks and water-borne coatings, in acrylic emulsion, improves its adhesiveproperties.
Embodiment
Below be described in further detail but embodiment and do not mean that limitation of the invention by specific examples; Among following each embodiment, related parts by weight all are with listed as parts by weight except as otherwise noted.
Embodiment 1: the methyl esters of rosin emulsion is the preparation of viscous liquid
46 parts of methyl esters of rosin are added in the emulsifying kettle, be heated to 50 ℃ ~ 60 ℃, the emulsifying agent B that under agitation adds successively 3 parts of emulsifying agent A and 0.5 part, stir, the deionized water that slowly adds 5.5 parts 50 ℃ ~ 60 ℃ with 20 ~ 25 minutes times carries out emulsification, emulsifying temperature is controlled at 50 ℃ ~ 60 ℃, and mixing speed is controlled at 80 ~ 110 rev/mins; Then, add 40.5 parts 50 ℃ ~ 60 ℃ deionized water, rotating speed progressively is reduced to 50 rev/mins again, until till mixing fully, whole emulsification times is controlled at 40 minutes; At last the gained emulsion is namely got product after filtration.
The solid content of measuring product is 52 ± 2%, and median size is less than 0.5 μ m, and viscosity is less than 200mPa.s.
Embodiment 2: softening temperature is the preparation of 45 ℃ flexalyn emulsion
46 parts of flexalyns are added in the emulsifying kettle, be heated to 50 ℃ ~ 60 ℃, the emulsifying agent B that under agitation adds successively 3 parts of emulsifying agent A and 0.5 part, stir, the deionized water that slowly adds 18.5 parts 50 ℃ ~ 60 ℃ with 40 ~ 50 minutes times carries out emulsification, emulsifying temperature is controlled at 50 ℃ ~ 60 ℃, mixing speed is controlled at 80 ~ 110 rev/mins, then, the deionized water that adds again 28 parts 50 ℃ ~ 60 ℃, rotating speed progressively is reduced to 50 rev/mins, until till mixing fully, whole emulsification times is controlled at 60 minutes, at last the gained emulsion is namely got product after filtration.
The solid content of measuring product is 52 ± 2%, and median size is less than 0.5 μ m, and viscosity is less than 200mPa.s.
Embodiment 3: softening temperature is 70 ℃ ~ 85 ℃ and is the preparation of rosin ethylene glycol ester, glyceryl ester, pentaerythritol ester and their mixed ester emulsion
46 parts of rosin resins are added in the emulsifying kettle, be heated to 120 ℃ ~ 125 ℃, the emulsifying agent B that under agitation adds successively 3.2 parts of emulsifying agent A and 0.9 part, stir, when temperature of charge is down to 115 ℃ ~ 118 ℃ in the still, the deionized water that begins to drip 18.5 parts 90 ℃ ~ 100 ℃ with 40 ~ 50 minutes times carries out emulsification, emulsifying temperature is controlled at 90 ℃ ~ 99 ℃, mixing speed is controlled at 80 ~ 110 rev/mins, then, add 28 parts 90 ℃ ~ 100 ℃ deionized water, rotating speed progressively is reduced to 50 rev/mins again, until till mixing fully, whole emulsification times is controlled at 60 minutes; At last the gained emulsion is cooled to below 60 ℃, namely gets after filtration product.
Measure the solid content 52 ± 2% of product, median size is less than 0.5 μ m, and viscosity is less than 200mPa.s.
Embodiment 4: softening temperature is the preparation of 90 ℃ ~ 95 ℃ glycerin abietate modified and pentaerythritol esters and their mixed ester emulsion
Above 46 parts of rosin resins are added in the emulsifying kettle, are heated to 120 ℃ ~ 125 ℃, under agitation add successively the emulsifying agent B of 3.2 parts of emulsifying agent A and 0.9 part, stir.When temperature of charge was down to 115 ℃ ~ 118 ℃ in the still, the deionized water that begins to drip 18.5 parts 95 ℃ ~ 100 ℃ with 40 ~ 50 minutes times carried out emulsification, and emulsifying temperature is controlled at 95 ℃ ~ 99 ℃, and mixing speed is controlled at 80 ~ 110 rev/mins.Then, add 28 parts 95 ℃ ~ 100 ℃ deionized water, rotating speed progressively is reduced to 50 rev/mins again, until till mixing fully, whole emulsification times is controlled at 60 minutes, at last the gained emulsion is cooled to below 60 ℃, namely gets after filtration product.
The solid content of measuring product is 52 ± 2%, and median size is less than 0.5 μ m, and viscosity is less than 200mPa.s.
Embodiment 5: softening temperature is the preparation of the mixed ester emulsion of 100 ℃ ~ 110 ℃ modification maleated rosin esters, polymerized rosin ester and they and low softening point rosin ester
Above 46 parts of rosin resins are added in the emulsifying kettle, are heated to 120 ℃ ~ 125 ℃, under agitation add successively the emulsifying agent B of 3.2 parts of emulsifying agent A and 0.9 part, stir.When temperature of charge is down to 115 ℃ ~ 118 ℃ in the still, the deionized water that begins to drip 18.5 parts 98 ℃ ~ 100 ℃ with 40 ~ 50 minutes times carries out emulsification, emulsifying temperature is controlled at 95 ℃ ~ 99 ℃, and mixing speed is controlled at 80 ~ 110 rev/mins, then, the deionized water that adds again 28 parts 98 ℃ ~ 100 ℃, rotating speed progressively is reduced to 50 rev/mins, until till mixing fully, whole emulsification times is controlled at 60 minutes, at last the gained emulsion is cooled to below 60 ℃, namely gets after filtration product.
Measure the solid content 52 ± 2% of product, median size is less than 0.5 μ m, and viscosity is less than 200mPa.s.
Claims (4)
1. the preparation method of a water base Gum Rosin Tackified emulsion, its making method comprises the steps:
A, Gum Rosin is added in the emulsifying kettle, is heated to the temperature that exceeds 5 ℃ ~ 50 ℃ of its softening temperatures, under agitation add successively mass concentration and be 6% ~ 10% emulsifying agent A and 1% ~ 4% emulsifying agent B, stir;
B, the deionized water that accounts for Gum Rosin weight 10% ~ 40% that slowly adds through preheating in A step gains carry out emulsification, and the emulsifying temperature of deionized water temperature and Gum Rosin is close, 80 to turn ~ 110 rev/mins speed stirring; Add synthermal deionized water again, reduce mixing speed to 50 rev/min, until mix fully, whole emulsification times is 40 minutes ~ 60 minutes;
C, B step gained emulsion is cooled below 60 ℃, filter, namely get this water base Gum Rosin Tackified emulsion.
2. the preparation method of water base Gum Rosin Tackified emulsion according to claim 1 is characterized in that:
In the above-mentioned B step, 90 ℃ ~ 100 ℃ of the emulsifying temperatures of high-softening-point rosin resin, 95 ~ 100 ℃ of corresponding deionized water temperature; The emulsifying temperature of low softening point Gum Rosin is 50 ℃ ~ 70 ℃, 40 ~ 70 ℃ of corresponding deionized water temperature.
3. the preparation method of water base Gum Rosin Tackified emulsion according to claim 1 is characterized in that:
Among the step C, described emulsion is regulated its solid content with 80 ℃ ~ 100 ℃ deionized water before cooling.
4. it is characterized in that according to claim 1 and 2 or the preparation method of 3 described water base Gum Rosin Tackified emulsions:
Described Gum Rosin is the ester compound that makes of rosin and unit alcohol, dibasic alcohol or polyvalent alcohol generation esterification or their mixture; Unit alcohol is one or more mixtures in methyl alcohol, ethanol, propyl carbinol or the isooctyl alcohol; Dibasic alcohol is that ethylene glycol, Diethylene Glycol, glycol ether, triglycol or the polymerization degree are one or more mixtures in the polyoxyethylene glycol of 1-10; Polyvalent alcohol is one or more mixtures in glycerine, tetramethylolmethane, sorbyl alcohol or the sucrose.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104277623A (en) * | 2014-09-09 | 2015-01-14 | 安徽国电能源设备工程有限公司 | Rosin paint |
| CN105348544A (en) * | 2015-11-14 | 2016-02-24 | 广东华林化工有限公司 | Preparation method of rosin eater emulsion of small particle size |
| CN105860550A (en) * | 2016-05-12 | 2016-08-17 | 广西融水闽兴树脂有限公司 | Tackifier resin emulsion |
| CN105968832A (en) * | 2016-05-12 | 2016-09-28 | 广西融水闽兴树脂有限公司 | Preparation method for tackifying resin emulsion |
| CN106047214A (en) * | 2016-06-27 | 2016-10-26 | 广东科茂林产化工股份有限公司 | Rosin-based emulsifying agent and preparation method thereof |
| CN106496596A (en) * | 2016-12-05 | 2017-03-15 | 湘潭大学 | A kind of preparation method of rosin milk |
| CN106967367A (en) * | 2017-05-23 | 2017-07-21 | 汪建军 | A kind of Environment-friendlyadhesive adhesive and preparation method thereof |
| CN107325671A (en) * | 2017-06-20 | 2017-11-07 | 北京弘信润达装饰有限公司 | Slurry containing natural stone-powder and preparation method and application |
| CN107619642A (en) * | 2017-09-25 | 2018-01-23 | 广西众昌树脂有限公司 | The preparation method of liquid rosin resin |
| CN111892885A (en) * | 2020-08-18 | 2020-11-06 | 开化诚信树脂有限公司 | Liquid rosin tackifying resin and production method thereof |
| CN116333597A (en) * | 2023-02-15 | 2023-06-27 | 梁本武 | Reverse acidic coating and preparation method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104277623A (en) * | 2014-09-09 | 2015-01-14 | 安徽国电能源设备工程有限公司 | Rosin paint |
| CN105348544A (en) * | 2015-11-14 | 2016-02-24 | 广东华林化工有限公司 | Preparation method of rosin eater emulsion of small particle size |
| CN105348544B (en) * | 2015-11-14 | 2017-10-24 | 广东华林化工有限公司 | A kind of preparation method of small grain size rosin ester emulsion |
| CN105860550A (en) * | 2016-05-12 | 2016-08-17 | 广西融水闽兴树脂有限公司 | Tackifier resin emulsion |
| CN105968832A (en) * | 2016-05-12 | 2016-09-28 | 广西融水闽兴树脂有限公司 | Preparation method for tackifying resin emulsion |
| CN106047214B (en) * | 2016-06-27 | 2018-04-06 | 广东科茂林产化工股份有限公司 | A kind of gum rosin base emulsifier and preparation method thereof |
| CN106047214A (en) * | 2016-06-27 | 2016-10-26 | 广东科茂林产化工股份有限公司 | Rosin-based emulsifying agent and preparation method thereof |
| CN106496596A (en) * | 2016-12-05 | 2017-03-15 | 湘潭大学 | A kind of preparation method of rosin milk |
| CN106967367A (en) * | 2017-05-23 | 2017-07-21 | 汪建军 | A kind of Environment-friendlyadhesive adhesive and preparation method thereof |
| CN107325671A (en) * | 2017-06-20 | 2017-11-07 | 北京弘信润达装饰有限公司 | Slurry containing natural stone-powder and preparation method and application |
| CN107619642A (en) * | 2017-09-25 | 2018-01-23 | 广西众昌树脂有限公司 | The preparation method of liquid rosin resin |
| CN111892885A (en) * | 2020-08-18 | 2020-11-06 | 开化诚信树脂有限公司 | Liquid rosin tackifying resin and production method thereof |
| CN116333597A (en) * | 2023-02-15 | 2023-06-27 | 梁本武 | Reverse acidic coating and preparation method thereof |
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Application publication date: 20130206 |