CN103710153A - Method for rapid removal of phthalic acid ester compound in peppermint oil - Google Patents
Method for rapid removal of phthalic acid ester compound in peppermint oil Download PDFInfo
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- CN103710153A CN103710153A CN201310669113.6A CN201310669113A CN103710153A CN 103710153 A CN103710153 A CN 103710153A CN 201310669113 A CN201310669113 A CN 201310669113A CN 103710153 A CN103710153 A CN 103710153A
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- phthalate
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- spearmint oil
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Abstract
The invention discloses a method for rapid removal of a phthalic acid ester compound in peppermint oil. The method comprises the following steps: step (1), dissolving an alkali compound by adding water, and adding into the peppermint oil; and step (2), heating the peppermint oil, stirring, standing, separating an aqueous phase, after filtering an oil phase, washing to be neutral. After treatment by the method, the removal rate of the phthalic acid ester compound in the peppermint oil can maximize to reach more than 99%; and compared with other methods for removing a plasticizer, the method is simple and effective, and can greatly reduce the production cost.
Description
Technical field
The present invention relates to the removal technical field of fluidizer, specifically relate to a kind of removal method of phthalate compound.
Background technology
Phthalate refers to the esterified derivative of phthalic acid, is fluidizer the most common in plastic cement industry, adds in plastics to strengthen elasticity, transparency, wearing quality and work-ing life.Phthalate is daily and industrial being widely used, most widely used with di-2-ethylhexyl phthalate (DEHP), accounts for 3/4ths of fluidizer output, is secondly dibutyl phthalate (DBP).Existing experiment confirms that phthalate compound can shine into harm to children's liver and kidney, and can increase the probability that women suffers from breast cancer.At present, in the toy contacting with mouth that European Union has been used children and other articles for children, the content of phthalic ester has carried out strict restriction.
Spearmint oil be labiate peppermint or family peppermint fresh cauline leaf through distillable perfume oil, be colourless or flaxen clarified liq.In spearmint oil, principal constituent is levorotatory menthol, and content is about 62%-87%, and other compositions also have left-handed piperitone, isomenthone, pulegone, menthyl acetate etc.Because spearmint oil has the distinctive refrigerant breath of asia peppermint, be therefore widely used in food and daily use chemicals industry.In addition, spearmint oil also has very strong sterilization anti-microbial effect, uses and can play analgesia, antipruritic effect in external-applied ointment.
The method of existing removal fluidizer is less, and equipment investment amount is larger, is difficult for carrying out industrialization operation.As " the removal by radiation method of high density dimethyl phthalate " patent of publication number CN102219280A, the method of using energetic ray removal by radiation dimethyl phthalate is disclosed, therefore because this method needs high-energy radiation device, carry out industrialized feasibility not high." a kind of device of removing phthalate esters in drinking water " patent of publication number CN101654307A, disclose and used the devices such as ozone contact tower, ozonizer, mixed fillers reactor to remove the method for phthalic ester, the weak point of this method is that the device and the reactor that relate to are more, and industrial production drops into larger.
Summary of the invention
The invention provides the method for phthalate compound in a kind of quick removal spearmint oil, compare with other methods of removing fluidizer, this method is simply effective, and can significantly reduce production costs.
The present invention is achieved by the following technical solutions:
A method for phthalate compound in quick removal spearmint oil, comprises the following steps:
(1) alkaloid compound is dissolved in water, and joins in spearmint oil;
(2) spearmint oil is heated to 50-150 ℃, stirs, standing, water phase separated, after oil phase filters, washing is to neutral.
A kind of method of phthalate compound in quick removal spearmint oil, described phthalate comprises dimethyl phthalate (DMP), di-2-ethylhexyl phthalate (DEHP), dibutyl phthalate (DBP), diisobutyl phthalate (DIBP), diethyl phthalate (DEP), dinoctyl phthalate (DOP), dimixo-octyl phthalate (DIOP), the just own ester of phthalic acid two (DNHP), butyl phthalate benzene methyl (BBP), diisononyl phthalate (DINP), the mixing of one or more of Di Iso Decyl Phthalate (DIDP) etc.
A method for phthalate compound in quick removal spearmint oil, described alkaloid compound is one or more the mixing in sodium hydroxide, potassium hydroxide, calcium hydroxide, hydrated barta, zinc hydroxide, sodium carbonate, sodium phosphate.
A method for phthalate compound in quick removal spearmint oil, described alkaloid compound and the mass ratio of water are 1:2-1:20.
A method for phthalate compound in quick removal spearmint oil, described alkaloid compound and the mass ratio of phthalate compound are 1:1-20:1.
A method for phthalate compound in quick removal spearmint oil, described alkaloid compound and phthalate compound stirring reaction time are 0.5-12 hour.
Reaction formula of the present invention:
Advantage of the present invention is:
After processing by this method, in spearmint oil, phthalate compound clearance maximum can reach more than 98%, compares with other methods of removing fluidizer, and this method is simply effective, and can significantly reduce production costs.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art further to understand the present invention, but not limit in any form the present invention.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
embodiment 1
The present embodiment relates to the method for phthalate compound in a kind of quick removal spearmint oil, comprises the following steps:
Step (1), get 8 g sodium hydroxide, add water 16g, obtain solvent a;
Step (2), get spearmint oil 1000g(containing dibutyl phthalate 8000mg, content 0.8%), add after solution a, 50 ℃ of heating are stirred 0.5 hour, after removing water and get final product.
Detecting dibutyl phthalate content in spearmint oil is 5.5mg/kg, and clearance reaches 99.93%.
embodiment 2
The present embodiment relates to the method for phthalate compound in a kind of quick removal spearmint oil, comprises the following steps:
Step (1), get 20g sodium hydroxide, add water 400g, obtain solvent a;
Step (2), get spearmint oil 1000g(containing dimethyl phthalate 1000mg, content 0.1%), add after solution a, 150 ℃ of heating are stirred 12 hours, after removing water and get final product.
Detecting dimethyl phthalate content in spearmint oil is 1 mg/kg, and clearance reaches 99.9%.
embodiment 3
The present embodiment relates to the method for phthalate compound in a kind of quick removal spearmint oil, comprises the following steps:
Step (1), get 40g sodium hydroxide, add water 400g, obtain solvent a;
Step (2), get spearmint oil 1000g(containing di-2-ethylhexyl phthalate 5000mg, content 0.5%), add after solution a, 120 ℃ of heating are stirred 5 hours, after removing water and get final product.
Detecting di-2-ethylhexyl phthalate content in spearmint oil is 2.5mg/kg, and clearance reaches 99.95%.
Claims (6)
1. remove fast a method for phthalate compound in spearmint oil, it is characterized in that comprising the following steps:
(1) alkaloid compound is dissolved in water, and joins in spearmint oil;
(2) spearmint oil is heated to 50-150 ℃, stirs, standing, water phase separated, after oil phase filters, washing is to neutral.
2. the method for phthalate compound in a kind of quick removal spearmint oil according to claim 1, it is characterized in that, described phthalate comprises dimethyl phthalate (DMP), di-2-ethylhexyl phthalate (DEHP), dibutyl phthalate (DBP), diisobutyl phthalate (DIBP), diethyl phthalate (DEP), dinoctyl phthalate (DOP), dimixo-octyl phthalate (DIOP), the just own ester of phthalic acid two (DNHP), butyl phthalate benzene methyl (BBP), diisononyl phthalate (DINP), the mixing of one or more of Di Iso Decyl Phthalate (DIDP) etc.
3. the method for phthalate compound in a kind of quick removal spearmint oil according to claim 1, it is characterized in that, described alkaloid compound is one or more the mixing in sodium hydroxide, potassium hydroxide, calcium hydroxide, hydrated barta, zinc hydroxide, sodium carbonate, sodium phosphate.
4. the method for phthalate compound in a kind of quick removal spearmint oil according to claim 1, is characterized in that, described alkaloid compound and the mass ratio of water are 1:2-1:20.
5. the method for phthalate compound in a kind of quick removal spearmint oil according to claim 1, is characterized in that, described alkaloid compound and the mass ratio of phthalate compound are 1:1-20:1.
6. the method for phthalate compound in a kind of quick removal spearmint oil according to claim 1, is characterized in that, described alkaloid compound and phthalate compound stirring reaction time are 0.5-12 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310669113.6A CN103710153A (en) | 2013-12-11 | 2013-12-11 | Method for rapid removal of phthalic acid ester compound in peppermint oil |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310669113.6A CN103710153A (en) | 2013-12-11 | 2013-12-11 | Method for rapid removal of phthalic acid ester compound in peppermint oil |
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| CN103710153A true CN103710153A (en) | 2014-04-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201310669113.6A Pending CN103710153A (en) | 2013-12-11 | 2013-12-11 | Method for rapid removal of phthalic acid ester compound in peppermint oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107790066A (en) * | 2016-09-05 | 2018-03-13 | 丰益(上海)生物技术研发中心有限公司 | The method for reducing content of plasticizing agent in raw material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304418A (en) * | 2011-07-26 | 2012-01-04 | 中山大学 | Method of removing polluted phthalate ester material from animal and plant essential oil |
| CN102586022A (en) * | 2012-01-12 | 2012-07-18 | 中山大学 | Method for removing plasticizer in plant essential oil |
-
2013
- 2013-12-11 CN CN201310669113.6A patent/CN103710153A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304418A (en) * | 2011-07-26 | 2012-01-04 | 中山大学 | Method of removing polluted phthalate ester material from animal and plant essential oil |
| CN102586022A (en) * | 2012-01-12 | 2012-07-18 | 中山大学 | Method for removing plasticizer in plant essential oil |
Non-Patent Citations (3)
| Title |
|---|
| 丁志彬等: "邻苯二甲酸酯类增塑剂水解条件的研究", 《包装工程》, vol. 31, no. 13, 31 December 2010 (2010-12-31) * |
| 孙清华等: "薄荷油中邻苯二甲酸酯类增塑剂的快速鉴别方法", 《香料香精化妆品》, no. 5, 31 October 2012 (2012-10-31) * |
| 莱伯泰科有限公司: "含油食品中塑化剂的GPC净化分析", 《食品安全导刊》, no. 07, 31 July 2011 (2011-07-31), pages 32 - 33 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107790066A (en) * | 2016-09-05 | 2018-03-13 | 丰益(上海)生物技术研发中心有限公司 | The method for reducing content of plasticizing agent in raw material |
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Application publication date: 20140409 |