CN102978010A - Process method for producing epoxidized soybean oil by using crude soybean oil as raw material - Google Patents
Process method for producing epoxidized soybean oil by using crude soybean oil as raw material Download PDFInfo
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Abstract
The invention provides a method for producing epoxidized soybean oil by using crude soybean oil as a raw material. The method is characterized by comprising the following steps of: 1, mixing four grades of crude soybean oil with phosphoric acid, settling until separation of oil foots, removing the remaining phospholipid from an oil layer through membrane treatment, then raising the temperature to be between 50 and 90 DEG C, keeping the temperature constant for 10 to 30 minutes, cooling and mixing with thin lye, and after mixing, keeping the temperature of the system constant at 100 DEG C for 45 minutes and then performing centrifugal separation to obtain treated crude soybean oil; and 2, under a microwave condition, dripping urea peroxide into the oil obtained in the step 1 for epoxidation, neutralizing the mixture with thin lye, performing water-washing, separating the oil from the water, and dehydrating to obtain finished epoxidized soybean oil. The epoxide number of the finished epoxidized soybean oil obtained by the method can be between 6.0 and 6.5 and the acid number is reduced to be below 0.6 mgKOH/g.
Description
Technical field
The present invention relates to a kind of take the method for crude oil of soybean as the raw material production epoxy soybean oil.
Background technology
Epoxy soybean oil is domestic and international Application and Development a kind of epoxy plasticizer early, have good thermostability, light stability, water tolerance and oil-proofness, developed into the third-largest class softening agent, be widely used in the goods such as nontoxic PVC film, drug packages, plastic door-window, tubing, house decorative material, electric wire, medical apparatus, toy for children, cultural goods.
Prior art all with the purified soyabean oil of environmental protection as the main raw of producing epoxy soybean oil, thereby production cost is very high.For reducing production costs, increase the competitive capacity in market, seek cheaply that raw materials for production substitute purified soyabean oil, become the research and development merit pass problem of respectively producing epoxy soybean oil producer.
Summary of the invention
The objective of the invention is to provide a kind of method of producing epoxy soybean oil with crude oil of soybean, cost is low, and technique is simple, and operational safety can satisfy commercial scale production.
In order to achieve the above object, the invention provides and a kind ofly it is characterized in that take the method for crude oil of soybean as the raw material production epoxy soybean oil concrete steps are:
The first step: be that 85% phosphoric acid mixes 1～10min with level Four crude oil of soybean and concentration, the phosphoric acid consumption is the 0.2%-2% of crude oil of soybean weight, mixing temperature is 20～50 ℃, sedimentation removed the sub-cloud soap stock in 2 hours, supernatant liquid is warming up to 50～90 ℃ after removing residue phosphatide by the film processing, insulation 10～30min, then be cooled to 20～50 ℃, be that rare potassium hydroxide aqueous solution of 5～20Be ' mixes acid value is dropped to below 1 with concentration again, be heated to 100 ℃, insulation 45min enters at last the butterfly centrifugal machine and separates the crude oil of soybean that obtains processing;
Second step: under microwave condition, drip concentration in the crude oil of soybean that obtains to the first step and be 10% urea peroxide solution and carry out epoxy reaction, the add-on of urea peroxide solution be oily heavy by 40%, and temperature is controlled at 50-100 ℃, reacts 4-10 hour;
The 3rd step: be the dilute alkaline soln neutralization of 1-10Be ' with the reaction product concentration of second step gained, wash, oily water separation, decompression dehydration obtains the finished product epoxy soybean oil again.
The oxirane value of the resulting finished product epoxy soybean oil of the present invention can reach 6.0-6.5, and acid number drops to below the 0.6mgKOH/g.
Compared with prior art, advantage of the present invention is:
1, the present invention is take the level Four crude oil of soybean as raw material, and the film handling oil can make wherein phospholipids content be down to below the 10ppm, more is conducive to the carrying out of epoxidation reaction.
2, urea peroxide has stronger reactive behavior, can impel the carrying out of epoxidation reaction.The oxirane value of finished product epoxy soybean oil of the present invention can reach 6.0-6.5, and acid number drops to below the 0.6mgKOH/g.
Embodiment
Further specify the present invention below in conjunction with embodiment.Among each embodiment, the testing method that acid number adopts adopts the mensuration of GB/T1668-2008 softening agent acid number and acidity, and the testing method of oxirane value adopts the mensuration of GB/T 1677-2008 softening agent oxirane value.
Embodiment 1
A kind of take the method for crude oil of soybean as the raw material production epoxy soybean oil, specific as follows:
(1) (iodine number is 128% to raw material level Four crude oil of soybean, acid number 1.3mgKOH/g) adding oil in, to weigh 0.3% concentration be 85% phosphoric acid solution, sedimentation 2h was except the sub-cloud oil foot after temperature remained on 50 ℃ of lower 10min of mixing, supernatant liquid is processed to remain by film and is warming up to 80 ℃ after phosphatide is removed, and constant temperature 30min, then be cooled to 50 ℃, and mix with rare potassium hydroxide aqueous solution and to make acid value reduce to 0.8, concentration of lye is 15Be ', the alkali lye consumption calculates according to acid value, and calculation formula is: actual alkali charge=oil weight * acid value * 1.3 * 10
-3/ alkali lye massfraction rises to 100 ℃ of insulation 45min with mixeding liquid temperature, enters at last the butterfly centrifugal machine and separates the crude oil of soybean that obtains processing;
(2) under microwave condition (power is 648W), dripping in batches concentration in the crude oil of soybean that obtains to the first step is the 10% urea peroxide aqueous solution, the add-on of urea peroxide solution is that oil is heavy by 40%, and this epoxy reaction temperature is controlled at 80 ℃, 10 hours time;
(3) be the sodium hydroxide solution neutralization of 10Be ' with the reaction product concentration of gained, be neutrality to water layer till, washing, dehydration obtains the finished product epoxy soybean oil, products obtained therefrom oxirane value 6.1%, acid number 0.6mgKOH/g, color and luster 160# (platinum cobalt colorimetry).
Embodiment 2
A kind of take the method for crude oil of soybean as the raw material production epoxy soybean oil, specific as follows:
(1) (iodine number is 128% to raw material level Four crude oil of soybean, acid number 1.3mgKOH/g) adding oil in, to weigh 0.3% concentration be 85% phosphoric acid solution, sedimentation 2h was except the sub-cloud oil foot after temperature remained on 50 ℃ of lower 10min of mixing, supernatant liquid is processed to remain by film and is warming up to 90 ℃ after phosphatide is removed, and constant temperature 30min, then be cooled to 50 ℃, and mix with rare potassium hydroxide aqueous solution and to make acid value reduce to 0.8, concentration of lye is 20Be ', the alkali lye consumption calculates according to acid value, and calculation formula is: actual alkali charge=oil weight * acid value * 1.3 * 10
-3/ alkali lye massfraction rises to 100 ℃ of insulation 45min with mixeding liquid temperature, enters at last the butterfly centrifugal machine and separates the crude oil of soybean that obtains processing;
(2) under microwave condition (power is 648W), drip in batches concentration in the crude oil of soybean that obtains to the first step and be 10% the urea peroxide aqueous solution, the add-on of urea peroxide solution is that oil is heavy by 40%, and this epoxy reaction temperature is controlled at 90 ℃, 10 hours time;
(3) be the sodium hydroxide solution neutralization of 10Be ' with the reaction product concentration of gained, be neutrality to water layer till, washing, dehydration obtains the finished product epoxy soybean oil, products obtained therefrom oxirane value 6.5%, acid number 0.6mgKOH/g, color and luster 130# (platinum cobalt colorimetry).
Embodiment 3
A kind of take the method for crude oil of soybean as the raw material production epoxy soybean oil, specific as follows:
(1) (iodine number is 128% to raw material level Four crude oil of soybean, acid number 1.3mgKOH/g) adding oil in, to weigh 0.3% concentration be 85% phosphoric acid solution, sedimentation 2h was except the sub-cloud oil foot after temperature remained on 30 ℃ of lower 10min of mixing, supernatant liquid is processed to remain by film and is warming up to 70 ℃ after phosphatide is removed, and constant temperature 30min, then be cooled to 20 ℃, and mix with rare potassium hydroxide aqueous solution and to make acid value reduce to 0.7, concentration of lye is 10Be ', the alkali lye consumption calculates according to acid value, and calculation formula is: actual alkali charge=oil weight * acid value * 1.3 * 10
-3/ alkali lye massfraction rises to 100 ℃ of insulation 45min with mixeding liquid temperature, enters at last the butterfly centrifugal machine and separates the crude oil of soybean that obtains processing;
(2) under microwave condition (power is 648W), drip in batches concentration in the crude oil of soybean that obtains to the first step and be 10% the urea peroxide aqueous solution, the add-on of urea peroxide solution is that oil is heavy by 40%, and this epoxy reaction temperature is controlled at 100 ℃, 6 hours time;
(3) be the sodium hydroxide solution neutralization of 10Be ' with the reaction product concentration of gained, be neutrality to water layer till, washing, dehydration obtains the finished product epoxy soybean oil, products obtained therefrom oxirane value 6.1%, acid number 0.6mgKOH/g, color and luster 130# (platinum cobalt colorimetry).
Embodiment 4
A kind of take the method for crude oil of soybean as the raw material production epoxy soybean oil, specific as follows:
(1) (iodine number is 128% to raw material level Four crude oil of soybean, acid number 1.3mgKOH/g) adding oil in, to weigh 0.3% concentration be 85% phosphoric acid solution, sedimentation 2h was except the sub-cloud oil foot after temperature remained on 50 ℃ of lower 10min of mixing, supernatant liquid is processed to remain by film and is warming up to 90 ℃ after phosphatide is removed, and constant temperature 10min, then be cooled to 50 ℃, and mix with rare potassium hydroxide aqueous solution and to make acid value reduce to 0.7, concentration of lye is 5Be ', the alkali lye consumption calculates according to acid value, and calculation formula is: actual alkali charge=oil weight * acid value * 1.3 * 10
-3/ alkali lye massfraction rises to 100 ℃ of insulation 45min with mixeding liquid temperature, enters at last the butterfly centrifugal machine and separates the crude oil of soybean that obtains processing;
(2) under microwave condition (power is 648W), drip in batches concentration in the crude oil of soybean that obtains to the first step and be 10% the urea peroxide aqueous solution, the add-on of urea peroxide solution is that oil is heavy by 40%, and this epoxy reaction temperature is controlled at 100 ℃, 10 hours time
(3) be the sodium hydroxide solution neutralization of 5Be ' with the reaction product concentration of gained, be neutrality to water layer till, washing, dehydration obtains the finished product epoxy soybean oil, products obtained therefrom oxirane value 6.3%, acid number 0.6mgKOH/g, color and luster 160# (platinum cobalt colorimetry).
Claims (1)
1. method of producing epoxy soybean oil take crude oil of soybean as raw material dirt is characterized in that concrete steps are:
The first step: be that 85% phosphoric acid mixes 1～10min with level Four crude oil of soybean and concentration, the phosphoric acid consumption is the 0.2%-2% of crude oil of soybean weight, mixing temperature is 20～50 ℃, sedimentation removed the sub-cloud soap stock in 2 hours, supernatant liquid is warming up to 50～90 ℃ after removing residue phosphatide by the film processing, insulation 10～30min, then be cooled to 20～50 ℃, be that rare potassium hydroxide aqueous solution of 5～20Be ' mixes acid value is dropped to below 1 with concentration again, be heated to 100 ℃, insulation 45min enters at last the butterfly centrifugal machine and separates the crude oil of soybean that obtains processing;
Second step: under microwave condition, drip concentration in the crude oil of soybean that obtains to the first step and be 10% urea peroxide solution and carry out epoxy reaction, the add-on of urea peroxide solution be oily heavy by 40%, and temperature is controlled at 50-100 ℃, reacts 4-10 hour;
The 3rd step: be the dilute alkaline soln neutralization of 1-10Be ' with the reaction product concentration of second step gained, wash, oily water separation, decompression dehydration obtains the finished product epoxy soybean oil again.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262297A (en) * | 2014-09-01 | 2015-01-07 | 南京工业大学 | Method for preparing high-quality epoxy vegetable oil by using microreactor |
| CN105254596A (en) * | 2015-09-18 | 2016-01-20 | 丹阳市助剂化工厂有限公司 | Preparation method for epoxidized soybean oil |
Citations (4)
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| JPH11158486A (en) * | 1997-11-27 | 1999-06-15 | Asahi Denka Kogyo Kk | Epoxidized animal or vegetable oil composition |
| CN101338042A (en) * | 2008-08-11 | 2009-01-07 | 浙江嘉澳化工有限公司 | Method for preparing biodegradable composite plasticiser |
| CN101591588A (en) * | 2009-06-24 | 2009-12-02 | 江南大学 | The method of organic rhenium oxide-urea peroxide catalytic preparation epoxy soybean oil or epoxyfatty acid first (second) ester |
| CN102250693A (en) * | 2011-06-21 | 2011-11-23 | 广州市新锦龙实业有限公司 | Process flow for preparing epoxidized soybean oil by using crude soybean oil |
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- 2012-12-03 CN CN201210512531.XA patent/CN102978010B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11158486A (en) * | 1997-11-27 | 1999-06-15 | Asahi Denka Kogyo Kk | Epoxidized animal or vegetable oil composition |
| CN101338042A (en) * | 2008-08-11 | 2009-01-07 | 浙江嘉澳化工有限公司 | Method for preparing biodegradable composite plasticiser |
| CN101591588A (en) * | 2009-06-24 | 2009-12-02 | 江南大学 | The method of organic rhenium oxide-urea peroxide catalytic preparation epoxy soybean oil or epoxyfatty acid first (second) ester |
| CN102250693A (en) * | 2011-06-21 | 2011-11-23 | 广州市新锦龙实业有限公司 | Process flow for preparing epoxidized soybean oil by using crude soybean oil |
Non-Patent Citations (3)
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| 施肖峰: "环氧大豆油及其生产工艺", 《中国油脂》, 2 March 1989 (1989-03-02), pages 48 - 51 * |
| 王维建等: "无溶剂一步法环氧棉籽油的合成", 《连云港化工高等专科学校学报》, vol. 12, no. 2, 30 June 1999 (1999-06-30), pages 31 - 33 * |
| 陈浩乾等: "绿色增塑剂环氧大豆油的开发与应用", 《广州化工》, vol. 36, no. 4, 31 December 2008 (2008-12-31), pages 6 - 8 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262297A (en) * | 2014-09-01 | 2015-01-07 | 南京工业大学 | Method for preparing high-quality epoxy vegetable oil by using microreactor |
| CN104262297B (en) * | 2014-09-01 | 2016-03-16 | 南京工业大学 | A kind of method adopting microreactor to prepare high-quality epoxidized vegetable oil |
| CN105254596A (en) * | 2015-09-18 | 2016-01-20 | 丹阳市助剂化工厂有限公司 | Preparation method for epoxidized soybean oil |
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