CN103058857A - Preparation method of disproportionated rosin potassium soap - Google Patents
Preparation method of disproportionated rosin potassium soap Download PDFInfo
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- CN103058857A CN103058857A CN2013100033087A CN201310003308A CN103058857A CN 103058857 A CN103058857 A CN 103058857A CN 2013100033087 A CN2013100033087 A CN 2013100033087A CN 201310003308 A CN201310003308 A CN 201310003308A CN 103058857 A CN103058857 A CN 103058857A
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Abstract
The invention relates to a preparation method of disproportionated rosin potassium soap, and provides a safe, environment-friendly, low-consumption, time-saving, low-production-cost disproportionated rosin potassium soap preparation method utilizing low temperature and normal pressure. The method comprises the steps of: potassium hydroxide dissolving, precipitating, preheating, saponification reaction, cooling, impurity removing, and canning.
Description
Technical field
The present invention relates to a kind of preparation method of disproportionated rosin potassium soap, be specifically related to a kind of preparation method of disproportionated rosin potassium soap.
Background technology
Disproportionated rosin potassium soap is emulsifying agent important in resin and the synthetic rubber, is a class rosin esterification derivative that utilizes two keys in the rosin acid structure and two chemical reactivity centers preparations of carboxyl.Color and thermostability are the leading indicators of its grade.The production of present domestic disproportionated rosin potassium soap mainly adopts the nilox resin of high-temperature fusion and potassium hydroxide alkali lye to carry out saponification reaction, the product that this traditional technique prepares, although substantially can satisfy the requirement of quality standard on the performance, but because the higher temperature (about 170 ℃) of reaction needed, so the input of equipment is larger, product colour is darker.Disproportionated rosin potassium soap ubiquity gel and crystalline polamer, the speed of letex polymerization and effect when having a strong impact on rubber production.For improving the color of product, can add the chemical assistants such as water glass, this method good decolorizing effect, but the speed of the existence of water glass letex polymerization rubber production can be affected the time.Someone improves gelatin phenomenon and the lamination problem of product by adding sodium-chlor, this method produces effect, but chloride content exceeds standard, and does not meet the quality product requirement.The somebody adopts staybelite Partial Replacement nilox resin, can effectively stop like this crystallization of product, but the technique more complicated needs to drop into larger cost.
Summary of the invention
Therefore, for above content, the invention provides a kind of safety, environmental protection, low consumption, save time, production cost is low, utilize low-temperature atmosphere-pressure to prepare the method for disproportionated rosin potassium soap.
For achieving the above object, the present invention is achieved by the following technical solutions: a kind of preparation method of disproportionated rosin potassium soap may further comprise the steps:
(1) dissolving of potassium hydroxide: potassium hydroxide is used deionized water dissolving at normal temperatures, obtain potassium hydroxide solution;
(2) precipitate: the potassium hydroxide solution after step (1) is handled staticly settles, and the throw out that obtains is removed the potassium hydroxide solution that obtains clarifying;
(3) preheating: the potassium hydroxide solution of the clarification that obtains after step (2) processed is sent into and is carried out preheating in the waste heat recovery tank;
(4) saponification reaction: then the potassium hydroxide of the clarification after the thermal pretreatment is sent into reactor is heated to 75～90 ℃, drops into nilox resin in reactor, carries out saponification reaction, and the temperature of reactor remains on 75～90 ℃, and the reaction times is controlled at 2～4 hours;
(5) cooling: the product after saponification reaction is complete is sent into water cooler, cools off;
(6) removal of impurity: the product after step (5) processing is sent into whizzer carry out centrifugal removal of impurities;
(7) enter tank: the product after will processing through whizzer enters tank, namely makes required disproportionated rosin potassium soap.
Further improve and be: the potassium hydroxide purity in the described step (1) is 95%.
Further improve and be: the solid content of the disproportionated rosin potassium soap of described step (7) is 25%.
Further improve and be: the consumption of the potassium hydroxide in the described step (1) is 4～6 weight parts, and the consumption of described deionized water is 73～77 weight parts, and the consumption of the nilox resin in the described step (4) is 19～21 weight parts.
Further improve and be: the solid content of the disproportionated rosin potassium soap of described step (7) is 50%.
Further improve and be: the consumption of the potassium hydroxide in the described step (1) is 8～12 weight parts, and the consumption of described deionized water is 47～53 weight parts, and the consumption of the nilox resin in the described step (4) is 39～41 weight parts.
Further improve and be: in the described step (1), in the dissolution process of potassium hydroxide, use stirrer to carry out stirring and dissolving, described deionization electrical conductivity of water＜10 μ s/cm, resistivity 〉=15M Ω.
By adopting the aforementioned techniques scheme, the invention has the beneficial effects as follows: the present invention is by adopting atmospheric low-temperature and control potassium hydroxide, nilox resin, deionized water three's ratio, the disproportionated rosin potassium soap quality index that makes all reaches LY/T1358-2008 very special quality standard, low 1-3 number of form and aspect bit-level standard, color is more shallow, and quality is good.Adopt the low temperature mode to produce, compare with traditional high temperature production mode, the production unit of input of the present invention is less, the electric energy of required consumption is also less, prepared product colour is more shallow, in addition, owing to the control of potassium hydroxide, nilox resin, deionized water three ratio and the control of saponification reaction time and temperature, effectively having avoided caking, a latch up phenomenon that occurs in the production process.
Embodiment
Describe embodiments of the present invention in detail below with reference to specific embodiment, how the utilisation technology means solve technical problem to the present invention whereby, and the implementation procedure of reaching technique effect can fully understand and implements according to this.
If do not specialize, the conventional means that the technique means that adopts among the embodiment is well known to those skilled in the art, the reagent that adopts and product also are and can commercial obtain.Various processes and the method described in detail are not ordinary methods as known in the art, and the source of agents useful for same, trade(brand)name and be necessary to list its moiety person are all indicated when occurring first.
Embodiments of the invention are:
A kind of preparation method of disproportionated rosin potassium soap take the disproportionated rosin potassium soap of preparation solid content as 25% as example, may further comprise the steps:
(1) dissolving of potassium hydroxide: be the deionized water dissolving that the potassium hydroxide of 95%, 5 weight parts is used 75 weight parts at normal temperatures with purity, use stirrer to carry out stirring and dissolving, obtain potassium hydroxide solution, described deionization electrical conductivity of water＜10 μ s/cm, resistivity 〉=15M Ω;
(2) precipitate: the potassium hydroxide solution after step (1) is handled staticly settles, and the throw out that obtains is removed the potassium hydroxide solution that obtains clarifying;
(3) preheating: the potassium hydroxide solution of the clarification that obtains after step (2) processed is sent into and is carried out preheating in the waste heat recovery tank;
(4) saponification reaction: then the potassium hydroxide of the clarification after the thermal pretreatment is sent into reactor is heated to 75～90 ℃, in reactor, drop into the nilox resin of 20 weight parts, carry out saponification reaction, the temperature of reactor remains on 75～90 ℃, and the reaction times is controlled at 2～4 hours;
(5) cooling: the product after saponification reaction is complete is sent into water cooler, cools off;
(6) removal of impurity: the product after step (5) processing is sent into whizzer carry out centrifugal removal of impurities,
(7) enter tank: the product after will processing through whizzer enters tank, namely obtains the K-25 disproportionated rosin potassium soap.
Wherein, nilox resin and the potassium hydroxide saponification reaction in the step (4) is as follows:
In the present invention, potassium hydroxide, nilox resin, the consumption of deionized water is to carry out regulating allocation according to the requirement of the solid content of the disproportionated rosin potassium soap that makes, potassium hydroxide in the present embodiment: nilox resin: deionized water=5:20:75, three's ratio is weight percentage, and when the solid content of required disproportionated rosin potassium soap is 50%, then only need the raising potassium hydroxide of corresponding proportion and the content of nilox resin, namely, at this moment, potassium hydroxide: nilox resin: deionized water=10:40:50, accordingly, if the preparation solid content is 60%, 80% disproportionated rosin potassium soap then changes corresponding ratio according to this principle and gets final product.
In addition, in the present invention, when the preparation solid content is 25% disproportionated rosin potassium soap, potassium hydroxide: nilox resin: deionized water=(4～6): (19～21): (73～77), when the nilox resin of preparation solid content when being 50%, potassium hydroxide: nilox resin: deionized water=(8～12): (39～41): (47～53), more than be mass percent, in this scope, all can realize purpose of the present invention.
The nilox resin that the present invention preferentially selects gloomy source, Yunnan chemical industry company limited to produce, the nilox resin that adopts other companies to produce can be realized purpose of the present invention equally.
Table 1 is the indices test result of disproportionated rosin potassium soap in the prior art, and table 2 is the indices test result of disproportionated rosin potassium soap of the present invention.
Table 1 raw material quality inspection report
Sample title: disproportionated rosin potassium soap
Table 2 raw material quality inspection report
Sample title: disproportionated rosin potassium soap
Contrast table 1 table 2 as can be known, form and aspect of the present invention number are than the form and aspect of prior art numbers low No. 3.
The disproportionated rosin potassium soap that utilizes the present invention to produce is estimated application test, method is as follows: according to SBR-1500,1502,1712 production formulas, the water for preparing (is comprised emulsifying agent, diffusant, ionogen and soft water etc.), activation phase solution, conditioning agent, vinylbenzene, oxygen scavengers etc. add in the polymeric kettle, with nitrogen replacement 3 times, after vacuumizing deoxygenation, add divinylic monomer, start polymerization kettle agitator, pass into water coolant to jacket of polymerization, when treating that the still temperature is cooled to polymeric reaction temperature (6 ± 0.5 ℃), add exciting agent solution, begin to count polymerization time.Keep polymeric reaction temperature constant, timing sampling is measured polymerisation conversion, when transformation efficiency reaches 30 ± 2%, add terminator, continue to stir and to guarantee to react completely terminations in 30 minutes, the final transformation efficiency of sampling survey, then discharging and obtain the glue sample through cohesion, washing, drying.
Carried out evaluation test to disproportionated rosin potassium soap at 15L intermittent type lab scale polymeric kettle device and 3 cubes of discontinuous emulsion polymerization pilot plants, the result shows:
(1) compare with the disproportionated rosin potassium soap that hot method is produced, utilize the lower temperature resistance of the disproportionated rosin potassium soap that the present invention prepares good, better mobile, colourity is better;
(2) polymerization process is steady, is easy to control, and speed of reaction is very fast;
(3) latex stable performance, the SBR-1500 of preparation, 1502,1712 product performance are better.
The present invention is by adopting atmospheric low-temperature and control potassium hydroxide, nilox resin, deionized water three's ratio, the K-25 disproportionated rosin potassium soap quality index that makes all reaches LY/T1358-2008 very special quality standard, low 1-3 number of form and aspect bit-level standard, color is more shallow, and quality is good.Adopt the low temperature mode to produce, compare with traditional high temperature production mode, the production unit of input of the present invention is less, the electric energy of required consumption is also less, prepared product colour is more shallow, in addition, owing to the control of potassium hydroxide, nilox resin, deionized water three ratio and the control of saponification reaction time and temperature, effectively having avoided caking, a latch up phenomenon that occurs in the production process.
The above record, only for utilizing the embodiment of this origination techniques content, modification, variation that any those skilled in the art use this creation to do all belong to the claim that this creation is advocated, and are not limited to those disclosed embodiments.
Claims (7)
1. the preparation method of a disproportionated rosin potassium soap is characterized in that, may further comprise the steps:
(1) dissolving of potassium hydroxide: potassium hydroxide is used deionized water dissolving at normal temperatures, obtain potassium hydroxide solution;
(2) precipitate: the potassium hydroxide solution after step (1) is handled staticly settles, and the throw out that obtains is removed the potassium hydroxide solution that obtains clarifying;
(3) preheating: the potassium hydroxide solution of the clarification that obtains after step (2) processed is sent into and is carried out preheating in the waste heat recovery tank;
(4) saponification reaction: then the potassium hydroxide of the clarification after the thermal pretreatment is sent into reactor is heated to 75～90 ℃, drops into nilox resin in reactor, carries out saponification reaction, and the temperature of reactor remains on 75～90 ℃, and the reaction times is controlled at 2～4 hours;
(5) cooling: the product after saponification reaction is complete is sent into water cooler, cools off;
(6) removal of impurity: the product after step (5) processing is sent into whizzer carry out centrifugal removal of impurities;
(7) enter tank: the product after will processing through whizzer enters tank, namely makes required disproportionated rosin potassium soap.
2. the preparation method of disproportionated rosin potassium soap according to claim 1, it is characterized in that: the potassium hydroxide purity in the described step (1) is 95%.
3. the preparation method of disproportionated rosin potassium soap according to claim 1 and 2, it is characterized in that: the solid content of the disproportionated rosin potassium soap of described step (7) is 25%.
4. the preparation method of disproportionated rosin potassium soap according to claim 3, it is characterized in that: the consumption of the potassium hydroxide in the described step (1) is 4～6 weight parts, the consumption of described deionized water is 73～77 weight parts, and the consumption of the nilox resin in the described step (4) is 19～21 weight parts.
5. the preparation method of disproportionated rosin potassium soap according to claim 1, it is characterized in that: the solid content of the disproportionated rosin potassium soap of described step (7) is 50%.
6. the preparation method of disproportionated rosin potassium soap according to claim 5, it is characterized in that: the consumption of the potassium hydroxide in the described step (1) is 8～12 weight parts, the consumption of described deionized water is 47～53 weight parts, and the consumption of the nilox resin in the described step (4) is 39～41 weight parts.
7. the preparation method of disproportionated rosin potassium soap according to claim 1, it is characterized in that: in the described step (1), in the dissolution process of potassium hydroxide, use stirrer to carry out stirring and dissolving, described deionization electrical conductivity of water＜10 μ s/cm, resistivity 〉=15M Ω.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103451050A (en) * | 2013-08-27 | 2013-12-18 | 广西梧州松脂股份有限公司 | Preparation method of light-color disproportionated rosin potash soap with 25% of solid content |
| CN103451051A (en) * | 2013-08-27 | 2013-12-18 | 广西梧州松脂股份有限公司 | Preparation method of disproportionated rosin potassium soap with solid content of 25 percent |
| CN103451049A (en) * | 2013-08-27 | 2013-12-18 | 广西梧州松脂股份有限公司 | Method for directly preparing disproportionated rosin potassium soap with solid content of 80 percent from solid disproportionated rosin |
| CN106118929A (en) * | 2016-06-29 | 2016-11-16 | 仇颖莹 | A kind of preparation method of tealeaf residue modification disproportionated rosin potassium soap |
| CN109232911A (en) * | 2018-10-09 | 2019-01-18 | 大同市恒源化工有限公司 | Neoprene emulsifier and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3012975A (en) * | 1958-05-01 | 1961-12-12 | Hercules Powder Co Ltd | Emulsifier for aqueous emulsion polymerization processes |
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2013
- 2013-01-06 CN CN2013100033087A patent/CN103058857A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3012975A (en) * | 1958-05-01 | 1961-12-12 | Hercules Powder Co Ltd | Emulsifier for aqueous emulsion polymerization processes |
Non-Patent Citations (1)
| Title |
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| 朱凯等: ""歧化松香钾皂的制备与性能"", 《精细化工》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103451050A (en) * | 2013-08-27 | 2013-12-18 | 广西梧州松脂股份有限公司 | Preparation method of light-color disproportionated rosin potash soap with 25% of solid content |
| CN103451051A (en) * | 2013-08-27 | 2013-12-18 | 广西梧州松脂股份有限公司 | Preparation method of disproportionated rosin potassium soap with solid content of 25 percent |
| CN103451049A (en) * | 2013-08-27 | 2013-12-18 | 广西梧州松脂股份有限公司 | Method for directly preparing disproportionated rosin potassium soap with solid content of 80 percent from solid disproportionated rosin |
| CN106118929A (en) * | 2016-06-29 | 2016-11-16 | 仇颖莹 | A kind of preparation method of tealeaf residue modification disproportionated rosin potassium soap |
| CN109232911A (en) * | 2018-10-09 | 2019-01-18 | 大同市恒源化工有限公司 | Neoprene emulsifier and preparation method thereof |
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Application publication date: 20130424 |