CN109554232A - A kind of preparation method of high-performance novel compounding wax - Google Patents
A kind of preparation method of high-performance novel compounding wax Download PDFInfo
- Publication number
- CN109554232A CN109554232A CN201811477532.9A CN201811477532A CN109554232A CN 109554232 A CN109554232 A CN 109554232A CN 201811477532 A CN201811477532 A CN 201811477532A CN 109554232 A CN109554232 A CN 109554232A
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- China
- Prior art keywords
- tree fat
- wax
- lacquer tree
- hydrogen
- reaction
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/12—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by hydrogenation
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B11/00—Recovery or refining of other fatty substances, e.g. lanolin or waxes
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention discloses a kind of preparation method of high-performance compounding wax, and preparation method includes the following steps: after weighing a certain amount of lacquer tree fat and hydrogenation catalyst, is placed in reaction kettle.After being passed through the hydrogen of certain pressure into kettle, temperature of reaction kettle is adjusted, after temperature reaches setting value, revolving speed knob is opened and carries out hydrogenation reaction and timing.After reaction, pressure in kettle is discharged, instrument is closed, carries out cooling processing.After being down to certain temperature, Filtration of catalyst obtains hydrofinishing lacquer tree fat.Hydrofinishing wax is compounded in proportion with Chinese vegetable tallow, carries out hydrofinishing according to the above method.After reaction, obtained novel built lacquer tree fat, iodine number is reduced to 8.74mg/g by original 22.36mg/g, fusing point is promoted to 52.9 DEG C by 48.2 DEG C, stearic acid content rises to 17.48% by original 5.77%, is better than hydrofinishing lacquer tree fat close to stearic acid content, the new wax performance after being compounded in Japan's purification Chinese wax, and cost has huge development prospect and the market competitiveness significantly lower than purification lacquer tree fat.
Description
Technical field
The present invention relates to chemosynthesis technical field, in particular to a kind of synthetic method of high-performance novel compounding wax.
Background technique:
Lacquer tree fat is important one of the forestry renewable biomass resources in China, from the fruit paint seed of lacquer tree.In recent years,
Mineral wax causes the safety problems such as intestinal cancer, all the time the extensive concern all by countries in the world.Therefore natural plants wax is opened
Hair research, becomes current optimal selection.Compared with mineral wax, natural plants wax majority is organism secretion in external progress
Self-protection substance or nutrient reserve, have no toxic and side effect to human body.Lacquer tree fat is exactly one kind of vegetable wax, it has good bullet
Property and flexibility, can be widely used in coating, daily cosmetics, electronic technology, textile printing and dyeing, superior cosmetics, medicine
Etc. industries, have a extensive future.Chinese tallow tree is also one of the characteristic tree species in China.By in the Chinese vegetable tallow prepared in the fruit of Chinese tallow tree
Palmitinic acid and oleic acid are mainly contained, can be used for manufacturing skin care oil, soap, paraffin paper, solid alcohol and fine perfumery, is a kind of good
Industrial chemicals.And the price of Chinese vegetable tallow is lower than lacquer tree fat, and Chinese vegetable tallow is compounded with lacquer tree fat, can prepare the new of low-cost and high-performance
Type haze tallow.
Chinese vegetable tallow and lacquer tree fat, this natural plants wax cause fusing point lower due to the presence of unsaturated bond, acid value iodine number
Higher, performance is unstable, is oxidized easily, and is unable to meet production demand, and storage transport is also more difficult.
Currently on the market using Japanese haze tallow as the high-performance lacquer tree fat of representative, application market is very well sold and in short supply, its price is it
5-8 times of allogene wax.And the lacquer tree fat processing technology backwardness that China is current, processing products obtained therefrom fusing point is low, color is deep, acid value
High, poor toughness, preparation be still low side crude product, limit in electronic product, ink material, the neck such as lubricant and brightener
The application in domain lacks the fine lacquer wax product of high added value.By hydrogen addition technology, the performance of natural plants wax can be improved, promoted
Fusing point reduces acid value iodine number.By adding hydrogen compounded technology, function admirable, inexpensive novel built wax, with this can also be obtained
Promote the market competitiveness and economic value.
Summary of the invention
A kind of preparation method of high-performance compounding wax, weighs the lacquer tree fat and hydrogenation catalyst (0.2%-0.35%) of 10g, sets
In high-temperature high-pressure reaction kettle, after being passed through the hydrogen (0.1-0.3MPa) of certain pressure, adjust temperature of reaction kettle (90-150 DEG C),
After reaction kettle reaches set temperature, turning knob is opened, is adjusted revolving speed (500r/min)；Start to carry out reaction timing (1-
3h), after reaction, gas reactor is discharged, revolving speed knob, cooling are closed；Resulting product will be reacted to be filtered, obtain essence
System plus hydrogen lacquer tree fat；Will plus hydrogen after lacquer tree fat and Chinese vegetable tallow (1: 1,1: 2,2: 1) compound according to certain proportion and add hydrogen, it is repeatedly above-mentioned
Step obtains high-performance compounding plus hydrogen lacquer tree fat.
Specific implementation method:
Embodiment 1
In hydrogenation conditions: catalyst amount 0.2%, Hydrogen Vapor Pressure 0.3MP, reaction time 1h, turn by 150 DEG C of reaction temperature
Under the conditions of fast 500r/min, selective hydrogenation catalyst: molybdenum trioxide, palladium carbon, Raney's nickel and rhodium carbon carry out hydrogenation reaction respectively.System
Obtain the purification lacquer tree fat of different content of fatty acid.Esterification is carried out to products therefrom: weighing the lacquer tree fat of 0.1g in test tube, is added
5mL n-hexane, 2mL 0.5% potassium hydroxide methanol solution after, clog test tube and shake up, until solution becomes clear.After clarification, separation
Out containing the supernatant liquor of methyl esters.Supernatant is subjected to GC-MS analysis.By comparing oleic acid in product and linoleic acid, stearic acid
The variation of content determines that palladium-carbon catalyst catalytic effect is best.
Embodiment 2
In hydrogenation conditions: Hydrogen Vapor Pressure 0.3Mpa, reaction time 2h, 150 DEG C of reaction temperature, revolving speed 500r/min, palladium carbon
Under conditions of catalyst amount respectively (0.2%, 0.35%, 0.5%), lacquer tree fat hydrogenation reaction is carried out, obtains purification lacquer tree fat.It is right
Products therefrom carries out esterification: weighing the lacquer tree fat of 0.1g in test tube, the potassium hydroxide first of 5mL n-hexane, 2mL 0.5% is added
It after alcoholic solution, clogs test tube and shakes up, until solution becomes clear.After clarification, the supernatant liquor containing methyl esters is isolated.By supernatant into
Row GC-MS analysis.By comparing the variation of oleic acid in product and linoleic acid, stearic acid content.After analyzing, catalyst amount is
When 0.5%, stearic acid relative amount reaches 17.44%, Japanese Chinese wax stearic acid relative amount in the content and document report
17.60% is close, so selecting 0.5% as catalyst amount.
Embodiment 3
With embodiment 2, Hydrogen Vapor Pressure is only changed to 0.1MPa, 0.2MPa, 0.3MPa, palladium-carbon catalyst dosage is
0.5%.Obtain purification lacquer tree fat.After analyzing, stearic acid content is most under conditions of pressure is 0.3MPa, in resulting lacquer tree fat
Height, so selection Hydrogen Vapor Pressure 0.3MPa is reacted.
Embodiment 4
With embodiment 3, only the reaction time it will be changed to 1h, 2h, 3h, and obtain purification lacquer tree fat.After analyzing, lacquer tree fat after 2h
Stearic acid relative amount is 24.34% after stearic acid content is 23.89%, 3h, and the two is not much different, overlong time, waste money
Source, thus select the reaction time for 2h.
Embodiment 5
With embodiment 4, reaction temperature is only changed to 90 DEG C, 120 DEG C, 150 DEG C, purification lacquer tree fat is made.After analyzing,
Under 150 DEG C of reaction conditions, stearic acid content has reached 23.22% in lacquer tree fat, and stearic acid content is significantly larger than at a temperature of 120 DEG C
Obtained purification lacquer tree fat stearic acid content 18.69%.Thus select 150 DEG C as optimal reaction temperature.
Embodiment 6
In palladium-carbon catalyst dosage 0.5%, Hydrogen Vapor Pressure 0.3Mpa, reaction time 2h, 150 DEG C of reaction temperature, 500r/
Under conditions of min, purification lacquer tree fat and LH wax are subjected to compounding plus hydrogen by 1: 2,1: 1,2: 1.Obtained purification compounding wax is divided
After analysis, stearic acid content reaches 17.48%, close to 17.60% in document report.It is tough compared with the lacquer tree fat after hydrofinishing
Property and plasticity be all superior to hydrogenation after lacquer tree fat, cost is also below the lacquer tree fat after hydrogenation.Before hydrogenating compared with lacquer tree fat, fusing point by
48.2 DEG C are improved to 52.9 DEG C, and iodine number, which is reduced, is reduced to 8.74mg/g by 22.36mg/g, and acid value is without significant change.For China's biology
Wax industry provides the novel raw material of function admirable.
The physical and chemical performance comparison of lacquer tree fat, Chinese vegetable tallow and compounding wax and Japanese Chinese wax before and after table 1 plus hydrogen
Certainly, the above description is not a limitation of the present invention, and the present invention is also not limited to the example above, the art
Ordinary person, within the essential scope of the present invention, variation, addition or the replacement made all should belong to protection model of the invention
It encloses.
Claims (3)
1. a kind of preparation method of high-performance novel compounding wax, implements as follows:
The first step weighs a certain amount of lacquer tree fat and hydrogenation catalyst, is placed in high-temperature high-pressure reaction kettle,
Second step after being passed through the hydrogen of certain pressure, adjusts temperature of reaction kettle,
Third step opens turning knob after reaction kettle reaches set temperature, adjusts revolving speed；
4th step starts to carry out reaction timing, after reaction, discharges gas reactor, closes revolving speed knob, cooling；
5th step will be reacted resulting product and is filtered, and purification plus hydrogen lacquer tree fat are obtained；
6th step will add after hydrogen lacquer tree fat compound according to certain proportion with Chinese vegetable tallow plus hydrogen, repeat the above steps, obtain high property
It can compounding plus hydrogen lacquer tree fat.
2. the preparation method of high-performance compounding wax according to claim 1, it is characterised in that second step and third step process
In, used method of hydrotreating is the mode that hydrogen is mended in segmentation.
3. the preparation method of high-performance according to claim 1 compounding wax, it is characterised in that the 6th step is by the paint after adding hydrogen
Wax carries out compounding by a certain percentage with Chinese vegetable tallow plus hydrogen, obtains the compounding wax of function admirable low cost.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811477532.9A CN109554232A (en) | 2018-11-30 | 2018-11-30 | A kind of preparation method of high-performance novel compounding wax |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811477532.9A CN109554232A (en) | 2018-11-30 | 2018-11-30 | A kind of preparation method of high-performance novel compounding wax |
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| Publication Number | Publication Date |
|---|---|
| CN109554232A true CN109554232A (en) | 2019-04-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811477532.9A Pending CN109554232A (en) | 2018-11-30 | 2018-11-30 | A kind of preparation method of high-performance novel compounding wax |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1138388A (en) * | 1965-09-20 | 1969-01-01 | British Petroleum Co | Improvements relating to the refining of wax |
| JPH02185595A (en) * | 1989-01-11 | 1990-07-19 | Noda Wax:Kk | Method for purifying and modifying crude wax |
| CN102329693A (en) * | 2011-08-12 | 2012-01-25 | 中国林业科学研究院林产化学工业研究所 | The preparation method of the meticulous article of a kind of high-quality lacquer tree fat |
| CN103804921A (en) * | 2013-12-26 | 2014-05-21 | 江西抚州国泰特种化工有限责任公司 | Novel plant mixed wax for explosive loading paper barrel |
-
2018
- 2018-11-30 CN CN201811477532.9A patent/CN109554232A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1138388A (en) * | 1965-09-20 | 1969-01-01 | British Petroleum Co | Improvements relating to the refining of wax |
| JPH02185595A (en) * | 1989-01-11 | 1990-07-19 | Noda Wax:Kk | Method for purifying and modifying crude wax |
| CN102329693A (en) * | 2011-08-12 | 2012-01-25 | 中国林业科学研究院林产化学工业研究所 | The preparation method of the meticulous article of a kind of high-quality lacquer tree fat |
| CN103804921A (en) * | 2013-12-26 | 2014-05-21 | 江西抚州国泰特种化工有限责任公司 | Novel plant mixed wax for explosive loading paper barrel |
Non-Patent Citations (2)
| Title |
|---|
| 裴曼琳 等: ""FT粗蜡的催化加氢精制"", 《石油化工》 * |
| 陈娆 等: ""复合油脂加氢生产植物蜡工艺的研究"", 《石油炼制与化工》 * |
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Application publication date: 20190402 |