CN108410584A - A kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer - Google Patents
A kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer Download PDFInfo
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- CN108410584A CN108410584A CN201810279643.2A CN201810279643A CN108410584A CN 108410584 A CN108410584 A CN 108410584A CN 201810279643 A CN201810279643 A CN 201810279643A CN 108410584 A CN108410584 A CN 108410584A
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- Prior art keywords
- rice bran
- fatty acid
- added
- medicine bottle
- plasticizer
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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
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/10—Applications used for bottles
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
In order to solve security risk existing for conventional plasticizers, the invention discloses a kind of medicine bottle preparation methods of natural rice bran fatty acid oil plasticizer.By refining rice bran oil aliphatic acid, esterification obtains natural plasticizer to the present invention in the presence of a catalyst with polyalcohol first, then after natural plasticizer being carried out epoxidation modification, purifies and separates are carried out using liquid-liquid extraction, revolving and freeze-drying obtain green safe and nontoxic medicine bottle rice bran oil fatty acid plasticizer after being further purified.With traditional plasticizer ratio, plastics tensile resistance prepared by the plasticizer of the preparation through the present invention is good.
Description
Technical field
The present invention relates to plasticizer field, the preparation side of specially a kind of medicine bottle natural rice bran fatty acid oil plasticizer
Method.
Background technology
World plastics industry is rapid, and purposes has penetrated into each department of national economy and each neck of people's life
Domain.Plastics have been listed as four big pillars of Material Field with steel, timber and cement.Various auxiliary agents in plastics are to improving plastics
The various performances of product play the role of extremely important.Plastic additive includes plasticizer, fire retardant, antioxidant and ultraviolet suction
Receive agent etc..Wherein plasticizer is a kind of maximum plastic additive of yield, and plasticizer industry is to promoting plastics industry especially polychlorostyrene
The development of ethylene industry plays conclusive effect.The plasticizer industry in China originates in later stage the 1950s, though starting
Late but development is very fast.The total output of China's industry plasticizer in 2005 oneself up to 1,600,000 tons, wherein adjacent benzene class plasticizer product accounts for master
Lead status.Studies have shown that this kind of plasticizer of Long Term Contact can endanger digestive system, increase the risk of angiocardiopathy, also
It can cause genotoxicity, or even cause cancer.Medicine bottle plays an important role to drug quality as drug storaging medium.If medicine
Product especially liquid medicine Long Term Contact Plastic medicinal bottle, the plasticizer in medicine bottle can be migrated into drug, will be brought to consumer sternly
The security risk of weight.Therefore, green non-poisonous plasticizer is researched and developed to have great importance.
Invention content
To solve the problems, such as traditional plasticizer, there are security risks, and the present invention provides a kind of medicine bottle natural rice oils extracted from rice husks
The preparation method of fatty acid plasticizer.
In order to realize that above-mentioned target, the present invention adopt the following technical scheme that：
A kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer, it is characterised in that include the following steps：
（1）The 2L rice bran oils refined are added to petroleum ether-ether in the mixed solvent of 10L, polyalcohol is added after stirring and dissolving
And after the KOH/methanol solution of 200ml saturations, be uniformly mixed, after reacting 1-2h at room temperature, 200-400ml water is added
After continue after stirring 5-10min, stand, after being layered, the rice bran oil that is esterified after taking upper layer that solvent is distilled off；
（2）Take 1L be esterified rice bran oil, be added 2L toluene dissolved after, alkanoic acid is added after the concentrated sulfuric acid of 18-20ml is added,
Hydrogen peroxide is slowly added dropwise under the conditions of 500-800rpm, after hydrogen peroxide adds, is warming up to 60-65 DEG C, carries out epoxidation reaction
After 6-10h, stop reaction, liquid temperature to be mixed reaches the ethyl acetate liquid-liquid extraction 2 times that 2L is added after room temperature, collects and merges second
Behind acetoacetic ester part, after the water that 100-200g anhydrous sodium sulfates remove in ethyl acetate is added, remaining part reduced pressure is distilled
Toluene and ethyl acetate are removed, finally obtains natural rice bran oil and fat by epoxidised rice bran oil fatty acid ester is freeze-dried
Sour plasticizer.
Preferably, step（1）Described in refined rice bran oil in contain 36% linoleic acid, 33% oleic acid, 22% palm fibre
Palmitic acid acid, 5% stearic acid and 4% leukotrienes.
Preferably, step（1）Described in petroleum ether-ether in the mixed solvent petroleum ether and ether volume ratio be 1：1.
Preferably, step（1）Described in polyalcohol be one kind in diethylene glycol (DEG) and monopropylene glycol, the addition of polyalcohol
Amount is the 10-20% of rice bran oil quality.
Preferably, step（2）Described in alkanoic acid be one kind in caproic acid or octanoic acid, the alkanoic acid addition be to be esterified
The 45-65% of rice bran oil.
Preferably, step（2）Described in hydrogen peroxide addition be esterification rice bran oil quality 100-150%.
Preferably, step（2）Described in vacuum distillation temperature be 45-50 DEG C.
Preferably, step（2）Described in freeze-drying temperature be-800-- 60 DEG C, sublimation drying 12-
18h。
A kind of preparation method of medicine bottle of the present invention natural rice bran fatty acid oil plasticizer has below beneficial to effect
Fruit：The present invention uses source of the natural rice bran oil as plasticizer, cheap and safe and non-toxic；Using polyalcohol to rice
After aliphatic acid in oil extracted from rice husks carries out esterification modification, the plasticising performance of rice bran oil fatty acid plasticizer is strengthened.It is found by comparing
The plasticizer that natural rice bran fatty acid oil plasticizer prepared by the present invention can replace traditional phthalate toxic.This
Outside, this law preparation process is simple, at low cost, and the plasticizer prepared through the present invention is safe and non-toxic, can be used as natural plasticizer
Applied in the preparation industry of medicine bottle plastics.
Specific implementation mode
Below with reference to specific embodiment to a kind of medicine bottle natural rice bran fatty acid oil plasticizer of the present invention
Preparation method is further elaborated, to help those skilled in the art to have more the inventive concept of the present invention, technical solution
Completely, accurate and deep understanding.
Embodiment 1
The 2L rice bran oils refined are added to petroleum ether-ether in the mixed solvent of 10L, be added after stirring and dissolving 15% it is two sweet
It after the saturation methanol solution of alcohol and 200ml KOH, is uniformly mixed, after reacting 2h at room temperature, it is subsequent that 300ml water is added
After continuous stirring 10min, stand, after being layered, the rice bran oil that is esterified after taking upper layer that solvent is distilled off；The rice for taking 1L to be esterified
Oil extracted from rice husks, be added 2L toluene dissolved after, be added after the concentrated sulfuric acid of 18ml after 40% caprylic acid is added, in 600rpm conditions
Under 35% hydrogen peroxide be slowly added dropwise after carrying out epoxidation reaction 10h after being warming up to 60 DEG C, stop anti-after hydrogen peroxide adds
It answers, liquid temperature to be mixed reaches the ethyl acetate liquid-liquid extraction 2 times that 2L is added after room temperature, after collecting combined ethyl acetate part,
After the water that 200g anhydrous sodium sulfates remove in ethyl acetate is added, remaining part is evaporated under reduced pressure under the conditions of 40 DEG C and removes first
After benzene and ethyl acetate, natural rice bran is obtained after dry 16h is lyophilized under the conditions of -75 DEG C in epoxidised rice bran oil fatty acid ester
Fatty acid oil plasticizer.
Embodiment 2
The 2L rice bran oils refined are added to petroleum ether-ether in the mixed solvent of 10L, single the third of 15% is added after stirring and dissolving
It after the saturation methanol solution of glycol and 200ml KOH, is uniformly mixed, after reacting 1.5h at room temperature, 500ml water is added
After continue after stirring 8min, stand, after being layered, the rice bran oil that is esterified after taking upper layer that solvent is distilled off；1L is taken to be esterified
Rice bran oil, be added 2L toluene dissolved after, be added after the concentrated sulfuric acid of 20ml after 45% caprylic acid is added, in 500rpm
Under the conditions of 30% hydrogen peroxide be slowly added dropwise after carrying out epoxidation reaction 8h after being warming up to 65 DEG C, stop after hydrogen peroxide adds
Reaction, liquid temperature to be mixed reach the ethyl acetate liquid-liquid extraction 2 times that 2L is added after room temperature, collect combined ethyl acetate part
Afterwards, after the water that 150g anhydrous sodium sulfates remove in ethyl acetate being added, remaining part is evaporated under reduced pressure under the conditions of 40 DEG C and is removed
After removing toluene and ethyl acetate, epoxidised rice bran oil fatty acid ester is lyophilized under the conditions of -70 DEG C after dry 16h and is obtained naturally
Rice bran oil fatty acid plasticizer.
Embodiment 3
The 2L rice bran oils refined are added to petroleum ether-ether in the mixed solvent of 10L, be added after stirring and dissolving 15% it is two sweet
It after the saturation methanol solution of alcohol and 200ml KOH, is uniformly mixed, after reacting 1.5h at room temperature, after 400ml water is added
Continue after stirring 10min, stands, after being layered, the rice bran oil that is esterified after taking upper layer that solvent is distilled off；1L is taken to be esterified
Rice bran oil, be added 2L toluene dissolved after, be added after the concentrated sulfuric acid of 20ml after 45% caproic acid is added, in 500rpm conditions
Under 30% hydrogen peroxide be slowly added dropwise after carrying out epoxidation reaction 10h after being warming up to 60 DEG C, stop anti-after hydrogen peroxide adds
It answers, liquid temperature to be mixed reaches the ethyl acetate liquid-liquid extraction 2 times that 2L is added after room temperature, after collecting combined ethyl acetate part,
After the water that 150g anhydrous sodium sulfates remove in ethyl acetate is added, remaining part is evaporated under reduced pressure under the conditions of 40 DEG C and removes first
After benzene and ethyl acetate, natural rice bran is obtained after dry 16h is lyophilized under the conditions of -70 DEG C in epoxidised rice bran oil fatty acid ester
Fatty acid oil plasticizer.
Performance test
After the polyvinyl resin of 400g is melted with tetrahydrofuran, embodiment 1,2, the plasticizer prepared by 3 and O-phthalic
After sour methyl esters mixing after blow molding process prepares film forming, measures its tensile strength and elongation at break is shown in Table 1
The tensile strength and elongation at break of polyethylene film prepared by the different plasticizer of table 1.
The stretch-proof of the plastic foil prepared as can be seen from the table with traditional plasticizer ratio, plasticizer prepared by the present invention
Intensity and elongation at break are good, can replace traditional plasticizer.
For the ordinary skill in the art, specific embodiment is only exemplarily described the present invention,
Obviously the present invention specific implementation is not subject to the restrictions described above, as long as use the inventive concept and technical scheme of the present invention into
The improvement of capable various unsubstantialities, or it is not improved by the present invention design and technical solution directly apply to other occasions
, in protection scope of the present invention.
Claims (8)
1. a kind of medicine bottle preparation method of natural rice bran fatty acid oil plasticizer, which is characterized in that include the following steps：
（1）The 2L rice bran oils refined are added to petroleum ether-ether in the mixed solvent of 10L, polyalcohol is added after stirring and dissolving
And after the KOH/methanol solution of 200ml saturations, be uniformly mixed, after reacting 1-2h at room temperature, 200-400ml water is added
After continue after stirring 5-10min, stand, after being layered, the rice bran oil that is esterified after taking upper layer that solvent is distilled off；
（2）Take 1L be esterified rice bran oil, be added 2L toluene dissolved after, alkanoic acid is added after the concentrated sulfuric acid of 18-20ml is added,
Hydrogen peroxide is slowly added dropwise under the conditions of 500-800rpm, after hydrogen peroxide adds, is warming up to 60-65 DEG C, carries out epoxidation reaction
After 6-10h, stop reaction, liquid temperature to be mixed, which reaches, the ethyl acetate of 2L is added after room temperature to be carried out liquid-liquid extraction 2 times, is collected simultaneously
After combined ethyl acetate phase, after the water that 100-200g anhydrous sodium sulfates remove in ethyl acetate is added, by remaining part reduced pressure
Toluene and ethyl acetate is distilled off, finally obtains natural rice oil extracted from rice husks by epoxidised rice bran oil fatty acid ester is freeze-dried
Fatty acid plasticizer.
2. a kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer according to claim 1, feature exist
In in step（1）Described in refined rice bran oil in containing 36% linoleic acid, 33% oleic acid, 22% palmitic acid, 5%
Stearic acid and 4% leukotrienes.
3. a kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer according to claim 1, feature exist
In in step（1）Described in petroleum ether-ether in the mixed solvent petroleum ether and ether volume ratio be 1：1.
4. a kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer according to claim 1, feature exist
In in step（1）Described in polyalcohol be one kind in diethylene glycol (DEG) and monopropylene glycol, the addition of polyalcohol is rice bran oil
The 10-20% of amount.
5. a kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer according to claim 1, feature exist
In in step（2）Described in alkanoic acid be one kind in caproic acid or octanoic acid, the alkanoic acid addition be the rice bran oil quality being esterified
45-65%.
6. a kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer according to claim 1, feature exist
In in step（2）Described in hydrogen peroxide addition be esterification rice bran oil quality 100-150%.
7. a kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer according to claim 1, feature exist
In in step（2）Described in vacuum distillation temperature be 45-50 DEG C.
8. a kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer according to claim 1, feature exist
In in step（2）Described in freeze-drying temperature be -80--60 DEG C, sublimation drying 12-18h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810279643.2A CN108410584A (en) | 2018-04-01 | 2018-04-01 | A kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810279643.2A CN108410584A (en) | 2018-04-01 | 2018-04-01 | A kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer |
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| Publication Number | Publication Date |
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| CN108410584A true CN108410584A (en) | 2018-08-17 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810279643.2A Pending CN108410584A (en) | 2018-04-01 | 2018-04-01 | A kind of preparation method of medicine bottle natural rice bran fatty acid oil plasticizer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115197198A (en) * | 2022-08-30 | 2022-10-18 | 汕头市龙琪塑料制品有限公司 | Preparation method of medicine bottle rice bran oil fatty acid plasticizer |
Citations (3)
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|---|---|---|---|---|
| CN101070510A (en) * | 2007-05-22 | 2007-11-14 | 李祥庆 | Method for producing epoxy plasticizer using waste grease |
| CN102503912A (en) * | 2011-10-26 | 2012-06-20 | 邹平福海科技发展有限公司 | High epoxide number environment-friendly plasticizer production process |
| CN105085982A (en) * | 2015-09-07 | 2015-11-25 | 四川大学 | Environment-friendly migration-resistant epoxy fatty acid cyclohexyl plasticizer and preparation method thereof |
-
2018
- 2018-04-01 CN CN201810279643.2A patent/CN108410584A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070510A (en) * | 2007-05-22 | 2007-11-14 | 李祥庆 | Method for producing epoxy plasticizer using waste grease |
| CN102503912A (en) * | 2011-10-26 | 2012-06-20 | 邹平福海科技发展有限公司 | High epoxide number environment-friendly plasticizer production process |
| CN105085982A (en) * | 2015-09-07 | 2015-11-25 | 四川大学 | Environment-friendly migration-resistant epoxy fatty acid cyclohexyl plasticizer and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 科技消息报: "米糠油制无毒包装增塑剂", 《中小企业科技信息》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115197198A (en) * | 2022-08-30 | 2022-10-18 | 汕头市龙琪塑料制品有限公司 | Preparation method of medicine bottle rice bran oil fatty acid plasticizer |
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Application publication date: 20180817 |
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