CN105062734A - Preparation method of disproportionated rosin potassium soap with solid content of 25% - Google Patents
Preparation method of disproportionated rosin potassium soap with solid content of 25% Download PDFInfo
- Publication number
- CN105062734A CN105062734A CN201510562123.9A CN201510562123A CN105062734A CN 105062734 A CN105062734 A CN 105062734A CN 201510562123 A CN201510562123 A CN 201510562123A CN 105062734 A CN105062734 A CN 105062734A
- Authority
- CN
- China
- Prior art keywords
- disproportionated rosin
- solid content
- reaction
- preparation
- solid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a preparation method of disproportionated rosin potassium soap with solid content of 25%, relating to the technical field of deep processing of rosin. The preparation method comprises the following steps: carrying out vacuum distillation on rosin to obtain refined rosin; then adding a palladium/carbon catalyst to carry out disproportionation reaction at the reaction temperature of 270-280 DEG C for 2.5-3.5 hours, and filtering for removing the palladium/carbon catalyst after the reaction, thereby obtaining solid disproportionated rosin; putting the obtained solid disproportionated rosin and a 45-50% potassium hydroxide solution into a reactor, reacting at 62-68 DEG C for 0.5-1 hour, then adding hydrogen peroxide and heating to 70-90 DEG C, and reacting for 0.5 hour, thereby obtaining the disproportionated rosin potassium soap with solid content of 25%. The preparation method of the disproportionated rosin potassium soap with solid content of 25% is more stable, safe and efficient in preparation process and low in production cost, and the prepared disproportionated rosin potassium soap with solid content of 25% has a light color.
Description
Technical field
The present invention relates to rosin deep process technology field, especially a kind of preparation method of solid content 25% disproportionated rosin potassium soap.
Background technology
Disproportionated rosin potassium soap is the kind that in rosin deep processed product, output is larger, is mainly used as the emulsifying agent of rubber.In China Synthetic Rubber Industry, emulsion polymerized styrene butadiene rubber, chloroprene rubber, paracril, ABS and butylbenzene/nitrile rubber all make emulsifying agent with disproportionated rosin potassium soap.Use nilox resin to make emulsifying agent the cohesive force of rubber can be made to strengthen, high-temperature capability raising, abrasion strength resistance and tearing toughness good, time mixing with natural rubber, adhesiveproperties has greatly improved.
But, not only there is potential safety hazard in preparation process to most of solid contents 25% disproportionated rosin potassium soap sold in the market, efficiency is low, production cost is high, also there is the darker problem of obtained product colour simultaneously, do not reach the standard of the market requirement, and from reducing the grade of its product.
Summary of the invention
The invention provides the preparation method of solid content 25% disproportionated rosin potassium soap that a kind of preparation process is more stable, safe, efficient, production cost is low, and product solid content 25% disproportionated rosin potassium soap that the method obtains is of light color.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
A kind of solid content 25% disproportionated rosin potassium soap, comprises following preparation process:
Gum resin vacuum distilling is obtained refining gum resin; Then add the disproportionation reaction that Pd/carbon catalyst carries out 2.5 ~ 3.5 hours, temperature of reaction is 270 DEG C ~ 280 DEG C, and reaction terminates rear mistake and filters Pd/carbon catalyst, obtains solid disproportionated rosin; The solid disproportionated rosin obtained first is put into reactor with the potassium hydroxide solution of 45% ~ 50%, react 0.5 ~ 1 hour at 62 DEG C ~ 68 DEG C, add hydrogen peroxide again and be warming up to 70 DEG C ~ 90 DEG C, reacting 0.5 hour, obtain this solid content 25% disproportionated rosin potassium soap;
The mass ratio of described solid disproportionated rosin, potassium hydroxide solution and hydrogen peroxide is: 2.8 ~ 3.1:1:0.002.
In technique scheme, scheme can also be more specifically: gum resin vacuum distilling is obtained refining gum resin; Then add the disproportionation reaction that Pd/carbon catalyst carries out 3 hours, temperature of reaction is 275 DEG C, and reaction terminates rear mistake and filters Pd/carbon catalyst, obtains solid disproportionated rosin; First putting into reactor with the potassium hydroxide solution of 48% by obtaining solid disproportionated rosin, reacting 0.5 hour at 65 DEG C, then add hydrogen peroxide and be warming up to 90 DEG C, reacting 0.5 hour, obtain this solid content 25% disproportionated rosin potassium soap;
The mass ratio of described solid disproportionated rosin and potassium hydroxide solution is: 3:1:0.002;
All N is led in described disproportionation reaction and saponification reaction process
2protection.
Owing to adopting technique scheme, the present invention has following beneficial effect:
1, owing to first being refined by gum resin, decrease the impurity in saponification reaction and by product, improve finished product transformation efficiency;
2, directly adopt solid resin to carry out saponification, gum resin melts and carries out with saponification reaction simultaneously, decreases the step and energy consumption of being melted by gum resin in advance, reduces production cost;
3, the saponification reaction time is shortened, the time of before being 1/3rd;
4, reduce operation easier, only need general technician can complete alone whole preparation process;
5, more stable, safe, efficient, thus improve the success ratio of preparation, reduce production cost;
6, the color of product is more shallow, and 25% disproportionated rosin potassium soap of gained directly surveys its Ghana's look number below 2 or 2, better quality.
7, adopt hydrogen peroxide as discoloring agent, it does not need additionally to carry out separating treatment after a procedure, but directly become water, can not bring any residual to stock product, and select hydrogen peroxide to be can not produce emulsifying materials and cause a large amount of bubbles, therefore be do not need to drop into emulsion splitter, only reaction product temperature of charge need be brought up to 70 ~ 90 DEG C, the a small amount of gas allowing the potash soap of high-content produce in whipping process naturally rises and drains, finally reach and reduce costs, improve the beneficial effect of the purity of product light color solid content 25% disproportionated rosin potassium soap.
Embodiment
Below in conjunction with specific examples, the invention will be further described:
Embodiment 1
Gum resin vacuum distilling is obtained refining gum resin; Then add the disproportionation reaction that Pd/carbon catalyst carries out 2.5 hours, temperature of reaction is 280 DEG C, and reaction terminates rear mistake and filters Pd/carbon catalyst, obtains solid disproportionated rosin; First putting into reactor with the potassium hydroxide solution of 48% by obtaining solid disproportionated rosin, reacting 0.5 hour at 62 DEG C, then add hydrogen peroxide and be warming up to 90 DEG C, reacting 0.5 hour, obtain this solid content 25% disproportionated rosin potassium soap;
The mass ratio of described solid disproportionated rosin and potassium hydroxide solution is: 2.8:1:0.002; All N is led in disproportionation reaction and saponification reaction process
2protection
Embodiment 2
Gum resin vacuum distilling is obtained refining gum resin; Then add the disproportionation reaction that Pd/carbon catalyst carries out 3 hours, temperature of reaction is 275 DEG C, and reaction terminates rear mistake and filters Pd/carbon catalyst, obtains solid disproportionated rosin; First putting into reactor with the potassium hydroxide solution of 45% by obtaining solid disproportionated rosin, reacting 0.5 hour at 65 DEG C, then add hydrogen peroxide and be warming up to 90 DEG C, reacting 0.5 hour, obtain this solid content 25% disproportionated rosin potassium soap;
The mass ratio of described solid disproportionated rosin and potassium hydroxide solution is: 3:1:0.002; All N is led in disproportionation reaction and saponification reaction process
2protection.
Embodiment 3
Gum resin vacuum distilling is obtained refining gum resin; Then add the disproportionation reaction that Pd/carbon catalyst carries out 3.5 hours, temperature of reaction is 270 DEG C, and reaction terminates rear mistake and filters Pd/carbon catalyst, obtains solid disproportionated rosin; First putting into reactor with the potassium hydroxide solution of 48% by obtaining solid disproportionated rosin, reacting 0.5 hour at 68 DEG C, then add hydrogen peroxide and be warming up to 90 DEG C, reacting 0.5 hour, obtain this solid content 25% disproportionated rosin potassium soap;
The mass ratio of described solid disproportionated rosin and potassium hydroxide solution is: 3.0:1:0.002; All N is led in disproportionation reaction and saponification reaction process
2protection.
Solid content 25% disproportionated rosin potassium soap technical indicator of the present invention is as table 1.
Table 1
。
Claims (3)
1. a preparation method for solid content 25% disproportionated rosin potassium soap, is characterized in that its preparation process is as follows:
Gum resin vacuum distilling is obtained refining gum resin; Then add the disproportionation reaction that Pd/carbon catalyst carries out 2.5 ~ 3.5 hours, temperature of reaction is 270 DEG C ~ 280 DEG C, and reaction terminates rear mistake and filters Pd/carbon catalyst, obtains solid disproportionated rosin; The solid disproportionated rosin obtained first is put into reactor with the potassium hydroxide solution of 45% ~ 50%, react 0.5 ~ 1 hour at 62 DEG C ~ 68 DEG C, add hydrogen peroxide again and be warming up to 70 DEG C ~ 90 DEG C, reacting 0.5 hour, obtain this solid content 25% disproportionated rosin potassium soap;
The mass ratio of described solid disproportionated rosin, potassium hydroxide solution and hydrogen peroxide is: 2.8 ~ 3.1:1:0.002.
2. the preparation method of solid content 25% disproportionated rosin potassium soap according to claim 1, is characterized in that its preparation process is as follows:
Gum resin vacuum distilling is obtained refining gum resin; Then add the disproportionation reaction that Pd/carbon catalyst carries out 3 hours, temperature of reaction is 275 DEG C, and reaction terminates rear mistake and filters Pd/carbon catalyst, obtains solid disproportionated rosin; First putting into reactor with the potassium hydroxide solution of 48% by obtaining solid disproportionated rosin, reacting 0.5 hour at 65 DEG C, then add hydrogen peroxide and be warming up to 90 DEG C, reacting 0.5 hour, obtain this solid content 25% disproportionated rosin potassium soap;
The mass ratio of described solid disproportionated rosin and potassium hydroxide solution is: 3:1:0.002.
3. the preparation method of solid content 25% disproportionated rosin potassium soap according to claim 1 and 2, is characterized in that all logical N in described disproportionation reaction and saponification reaction process
2protection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510562123.9A CN105062734A (en) | 2015-09-07 | 2015-09-07 | Preparation method of disproportionated rosin potassium soap with solid content of 25% |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510562123.9A CN105062734A (en) | 2015-09-07 | 2015-09-07 | Preparation method of disproportionated rosin potassium soap with solid content of 25% |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105062734A true CN105062734A (en) | 2015-11-18 |
Family
ID=54492256
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510562123.9A Pending CN105062734A (en) | 2015-09-07 | 2015-09-07 | Preparation method of disproportionated rosin potassium soap with solid content of 25% |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105062734A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109112021A (en) * | 2018-06-25 | 2019-01-01 | 广东科茂林产化工股份有限公司 | A kind of preparation method of disproportionated rosin potassium soap |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1613991A (en) * | 2004-09-16 | 2005-05-11 | 北京航空航天大学 | Decolouring refining process and apparatus for rosin soap |
| 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 |
-
2015
- 2015-09-07 CN CN201510562123.9A patent/CN105062734A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1613991A (en) * | 2004-09-16 | 2005-05-11 | 北京航空航天大学 | Decolouring refining process and apparatus for rosin soap |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109112021A (en) * | 2018-06-25 | 2019-01-01 | 广东科茂林产化工股份有限公司 | A kind of preparation method of disproportionated rosin potassium soap |
| CN109112021B (en) * | 2018-06-25 | 2021-03-30 | 广东科茂林产化工股份有限公司 | Preparation method of disproportionated rosin potassium soap |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102746793B (en) | Method for refining capsicum oleoresins | |
| CN103451051B (en) | Preparation method of disproportionated rosin potassium soap with solid content of 25 percent | |
| CN102558399B (en) | Preparation method of solvent-based tert-butyl peroxyneo-caprate with mass fraction of 75% | |
| CN104194641A (en) | Preparation method of hydrogenated rosin glyceride | |
| CN102070988A (en) | Method for producing water-white hydrogenated rosin | |
| CN102618072B (en) | Method for refining capsanthin by enzyme catalysis, esterification and molecular distillation | |
| CN105062734A (en) | Preparation method of disproportionated rosin potassium soap with solid content of 25% | |
| CN104531344A (en) | Method for producing walnut oil | |
| CN107501441A (en) | A kind of rubber production isproportionated potassium rosinate preparation method | |
| CN103451050B (en) | Preparation method of light-color disproportionated rosin potash soap with 25% of solid content | |
| CN104003962B (en) | A kind of preparation method and its usage of fucoxanthin | |
| CN102978050B (en) | Method for directly producing disproportionated rosin potassium soap with solid content of 25 percent | |
| CN102964314A (en) | Preparation method of epoxidized fatty acid methyl ester | |
| CN103013724B (en) | Production method for disproportionated rosin sodium soap | |
| CN103451049B (en) | Method for directly preparing disproportionated rosin potassium soap with solid content of 80 percent from solid disproportionated rosin | |
| CN106699624B (en) | A kind of production method of lutein | |
| CN103435473A (en) | Preparation method of light-colour disproportionated rosin potassium soap with solid content of 80% | |
| CN107183733A (en) | A kind of method for preparing capsicum seed oil and chilli seed dietary fiber | |
| CN105154271A (en) | Preparation method of disproportionated rosin potassium soap with light-color solid content of 25 percent | |
| CN106674152A (en) | Method for extracting accelerator M from waste resin | |
| CN105039029A (en) | Preparing method for disproportionated rosin potash soap with solid content of 80% | |
| CN102978051B (en) | Preparation method for disproportionated rosin potassium soap with solid content of 25% | |
| CN105039041A (en) | Preparation method of light-color disproportionated rosin potassium soap with solid content of 80% | |
| CN107312664A (en) | A kind of preparation method of disproportionated rosin sodium soap | |
| CN110684616A (en) | Preparation method of disproportionated rosin potassium soap with solid content of 25% |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20151118 |