CN103468316A - Preparation method of high-acid saponified oxidized wax - Google Patents
Preparation method of high-acid saponified oxidized wax Download PDFInfo
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- CN103468316A CN103468316A CN2013104743174A CN201310474317A CN103468316A CN 103468316 A CN103468316 A CN 103468316A CN 2013104743174 A CN2013104743174 A CN 2013104743174A CN 201310474317 A CN201310474317 A CN 201310474317A CN 103468316 A CN103468316 A CN 103468316A
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Abstract
The invention discloses a preparation method of high-acid saponified oxidized wax, which comprises the following steps: heating paraffin and microcrystalline wax to completely melt the paraffin and microcrystalline wax, respectively adding a catalyst and an assistant, and introducing oxygen at constant flow rate to react, wherein the catalyst is manganese acetate or manganese sulfate, the assistant is stearic acid, the reaction temperature is 130-180 DEG C, the reaction time is 1-7 hours, and the flow rate of oxygen is 50-110 mL/min. The acid value of the oxidized wax is 27.95 mg KOH/g, and the saponification value is 69.78 mg KOH/g. The preparation method has the advantages of simple technique, short reaction time and low reaction temperature, and is convenient to operate; and the prepared oxidized wax product has the advantages of light color, light smell and high saponification value.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of paraffin with the dioxygen oxidation melting, Microcrystalline Wax mixture to prepare the method for peracid soap oxidized petroleum waves.
Background technology
Paraffin is widely used in the fields such as food, medicine, detergents and cosmetic, leather, weaving as a kind of important Chemicals, and China is the big producing country of paraffin, but the paraffin wax product of China is mainly used in elementary traditional enterprise.Unprocessed paraffin viscosity is low, and snappiness is poor, is difficult to emulsification.Microcrystalline Wax is the chloroflo of separating in the residual oil from the underpressure distillation still, and its good luster, fusing point are high.Add a certain amount of Microcrystalline Wax in paraffin, can improve the performance of paraffin.
Use air or oxygen to carry out oxidation to molten wax, can in hydrocarbon, introduce polar functional group.Because variation has occurred for the structure of oxidized petroleum waves internal chain and surperficial character, its dissolving, emulsification, the performance such as lubricated have had great improvement.Therefore, oxidized petroleum waves have good emulsifying, oilness, pigment-dispersing, thereby enlarge its use range.
Chinese patent CN1206719A has reported the method by atmospheric oxidation Alathon and copolymer waxes, and the acid number of the oxidized petroleum waves that it prepares and saponification value are respectively 18mgKOH/g, 40mgKOH/g; Described the method for polyethylene wax Poly Propylene Wax and petroleum wax co-oxidation in the CN101082000A patent, the acid number of the oxidized petroleum waves that it prepares and saponification value can reach 29.6mgKOH/g, 56.8mgKOH/g; CN101289540A, CN101724107A have reported the method for oxidation of polyethylene wax or polythene wax emulsion, and less about the oxidation report of paraffin, Microcrystalline Wax.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of peracid soap oxidized petroleum waves, technique is simple, easy to operate, the reaction times is short, temperature of reaction is low, and the oxidized petroleum waves product color of preparation is shallow, smell is light, saponification value is high.
For achieving the above object, the present invention adopts following technical scheme:
A kind of preparation method of peracid soap oxidized petroleum waves makes its complete melting by the heating of paraffin and Microcrystalline Wax, adds respectively catalyzer and auxiliary agent, and the oxygen that passes into constant flow rate is reacted.
Described paraffin and Microcrystalline Wax are respectively 58# paraffin and 80# Microcrystalline Wax.
Take paraffin and Microcrystalline Wax as basic material, and the mass ratio of paraffin and Microcrystalline Wax is 8:2.
Described oxygen is pure, dry oxygen.
Type of heating is dimethyl silicone oil oil bath heating.
Described catalyzer is manganese acetate or manganous sulfate, preferably sulfuric acid manganese; Auxiliary agent is stearic acid; The quality of catalyzer is 0.52% of paraffin and Microcrystalline Wax total mass, and the quality of auxiliary agent is 12% of paraffin and Microcrystalline Wax total mass.
Temperature of reaction is 130 ~ 180 ℃, preferably 150 ℃.
Reaction times is 1 ~ 7h, preferably 5h.
Oxygen gas flow rate is 50 ~ 110mL/min, preferably 80mL/min.
Remarkable advantage of the present invention is: technique of the present invention is simple, easy to operate, the reaction times is short, temperature of reaction is low, and the oxidized petroleum waves product color of preparation is shallow, smell is light, saponification value is high.
Embodiment
The present invention relates to the preparation method of peracid soap oxidized petroleum waves, concrete steps are paraffin and the Microcrystalline Waxes that take the certain mass ratio, be added in three-necked flask, adopt the oil bath heating to make its complete melting, add catalyzer, auxiliary agent in batches, and pass into the dry oxygen of constant flow rate, reacted at a certain temperature.After the reaction certain hour, take out sample, moulding, measure its performance.
Below enumerate 5 embodiment, the present invention is described in further detail, but the present invention is not subject to the restriction of these embodiment.
Embodiment 1
Take paraffin and the Microcrystalline Wax of certain mass ratio, adopt oil bath heating three-necked flask, make its complete melting, under 140 ℃, take manganese acetate as catalyzer, stearic acid be auxiliary agent, the control oxygen gas flow rate is 80mL/min, oxidation 4h, after reaction finishes, take out sample, moulding, measure its performance, the results are shown in Table 1.
Table 1 manganese acetate catalyzed oxidation result
As can be seen from Table 1, when take manganese acetate as catalyzer, stearic acid during as auxiliary agent, the oxidized petroleum waves product acid number, the saponification value that obtain are lower, and color is darker.
Embodiment 2
Take manganous sulfate as catalyzer, and stearic acid is auxiliary agent, and method, with embodiment 1, the results are shown in Table 2.
Table 2 manganous sulfate catalyzed oxidation result
Comparison sheet 1 and table 2, under the same conditions, when take manganous sulfate as catalyzer, stearic acid during as auxiliary agent, the oxidized petroleum waves product acid number, the saponification value that obtain are higher, and color is more shallow.
Embodiment 3
Take paraffin and the Microcrystalline Wax of certain mass ratio, be added in three-necked flask, adopt the oil bath heating to make its complete melting, at a certain temperature, take manganous sulfate as catalyzer, stearic acid be auxiliary agent, the control oxygen gas flow rate is 80mL/min, and oxidation 4h, after reaction finishes, take out sample, moulding, measure its performance, the results are shown in Table 3.
The impact of table 3 temperature of reaction on oxidized petroleum waves character
Embodiment 4
Take paraffin and the Microcrystalline Wax of certain mass ratio, be added in three-necked flask, adopt the oil bath heating to make its complete melting, under 150 ℃, take manganous sulfate as catalyzer, stearic acid be auxiliary agent, the control oxygen gas flow rate is 80mL/min, after reaction for some time, take out sample, moulding, measure its performance, the results are shown in Table 4.
The impact of table 4 reaction times on oxidized petroleum waves character
Embodiment 5
Take paraffin and the Microcrystalline Wax of certain mass ratio, be added in three-necked flask, adopt the oil bath heating to make its complete melting, under 140 ℃, take manganous sulfate as catalyzer, stearic acid be auxiliary agent, control oxygen gas flow rate, oxidation 4h, after reaction finishes, take out sample, moulding, measure its performance, the results are shown in Table 5.
The impact of table 5 oxygen gas flow rate on oxidized petroleum waves character
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (9)
1. the preparation method of peracid soap oxidized petroleum waves is characterized in that: paraffin and Microcrystalline Wax heating are made to its complete melting, add respectively catalyzer and auxiliary agent, and the oxygen that passes into constant flow rate is reacted.
2. the preparation method of peracid soap oxidized petroleum waves according to claim 1, it is characterized in that: described paraffin and Microcrystalline Wax are respectively 58# paraffin and 80# Microcrystalline Wax.
3. the preparation method of peracid soap oxidized petroleum waves according to claim 1, it is characterized in that: take paraffin and Microcrystalline Wax as basic material, the mass ratio of paraffin and Microcrystalline Wax is 8:2.
4. the preparation method of peracid soap oxidized petroleum waves according to claim 1, it is characterized in that: described oxygen is pure, dry oxygen.
5. the preparation method of peracid soap oxidized petroleum waves according to claim 1 is characterized in that: type of heating is dimethyl silicone oil oil bath heating.
6. the preparation method of peracid soap oxidized petroleum waves according to claim 1, it is characterized in that: described catalyzer is manganese acetate or manganous sulfate, auxiliary agent is stearic acid, and the quality of catalyzer is 0.52% of paraffin and Microcrystalline Wax total mass, and the quality of auxiliary agent is 12% of paraffin and Microcrystalline Wax total mass.
7. the preparation method of peracid soap oxidized petroleum waves according to claim 1, it is characterized in that: temperature of reaction is 130 ~ 180 ℃.
8. the preparation method of peracid soap oxidized petroleum waves according to claim 1, it is characterized in that: the reaction times is 1 ~ 7h.
9. the preparation method of peracid soap oxidized petroleum waves according to claim 1, it is characterized in that: oxygen gas flow rate is 50 ~ 110mL/min.
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| CN2013104743174A CN103468316A (en) | 2013-10-12 | 2013-10-12 | Preparation method of high-acid saponified oxidized wax |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106010648A (en) * | 2016-07-13 | 2016-10-12 | 袁春华 | Method for preparing controllable shallow oxidized paraffin |
| CN109957425A (en) * | 2019-04-02 | 2019-07-02 | 周立华 | A kind of lacquer painting protection wax |
| CN112121740A (en) * | 2019-06-24 | 2020-12-25 | 内蒙古伊泰煤基新材料研究院有限公司 | Wax shallow oxidation method and device |
| CN115193363A (en) * | 2022-09-16 | 2022-10-18 | 世名(苏州)新材料研究院有限公司 | Oxidized wax with high acid value and low ester value, preparation process thereof and esterified wax prepared from oxidized wax |
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| GB787921A (en) * | 1954-06-11 | 1957-12-18 | South African Coal Oil Gas | Wax processing |
| GB902622A (en) * | 1958-07-23 | 1962-08-01 | British Petroleum Co | Improvements relating to the oxidation of residual petroleum waxes |
| GB902621A (en) * | 1958-07-23 | 1962-08-01 | British Petroleum Co | Improvements relating to the oxidation of residual petroleum waxes |
| CN1974730A (en) * | 2006-12-12 | 2007-06-06 | 刘俊生 | Process of producing oxygenated paraffin soap |
| CN102021034A (en) * | 2009-09-15 | 2011-04-20 | 中国石油天然气股份有限公司 | Preparation method of white microcrystalline wax |
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2013
- 2013-10-12 CN CN2013104743174A patent/CN103468316A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB787921A (en) * | 1954-06-11 | 1957-12-18 | South African Coal Oil Gas | Wax processing |
| GB902622A (en) * | 1958-07-23 | 1962-08-01 | British Petroleum Co | Improvements relating to the oxidation of residual petroleum waxes |
| GB902621A (en) * | 1958-07-23 | 1962-08-01 | British Petroleum Co | Improvements relating to the oxidation of residual petroleum waxes |
| CN1974730A (en) * | 2006-12-12 | 2007-06-06 | 刘俊生 | Process of producing oxygenated paraffin soap |
| CN102021034A (en) * | 2009-09-15 | 2011-04-20 | 中国石油天然气股份有限公司 | Preparation method of white microcrystalline wax |
Non-Patent Citations (3)
| Title |
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| 康蕾等: ""石蜡催化氧化反应热效应分析"", 《辽宁石油化工大学学报》 * |
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| 邓秀琴等: ""石蜡催化氧化反应的实现及催化作用"", 《辽宁石油化工大学学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106010648A (en) * | 2016-07-13 | 2016-10-12 | 袁春华 | Method for preparing controllable shallow oxidized paraffin |
| CN109957425A (en) * | 2019-04-02 | 2019-07-02 | 周立华 | A kind of lacquer painting protection wax |
| CN112121740A (en) * | 2019-06-24 | 2020-12-25 | 内蒙古伊泰煤基新材料研究院有限公司 | Wax shallow oxidation method and device |
| CN115193363A (en) * | 2022-09-16 | 2022-10-18 | 世名(苏州)新材料研究院有限公司 | Oxidized wax with high acid value and low ester value, preparation process thereof and esterified wax prepared from oxidized wax |
| CN115193363B (en) * | 2022-09-16 | 2023-02-24 | 世名(苏州)新材料研究院有限公司 | Oxidized wax with high acid value and low ester value, preparation process thereof and esterified wax prepared from oxidized wax |
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Application publication date: 20131225 |