CN111234920A - Refining method of castor oil with low acid value and low chroma - Google Patents

Refining method of castor oil with low acid value and low chroma Download PDF

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Publication number
CN111234920A
CN111234920A CN201911250436.5A CN201911250436A CN111234920A CN 111234920 A CN111234920 A CN 111234920A CN 201911250436 A CN201911250436 A CN 201911250436A CN 111234920 A CN111234920 A CN 111234920A
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China
Prior art keywords
castor oil
low
acid value
refining
adsorbent
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Pending
Application number
CN201911250436.5A
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Chinese (zh)
Inventor
胡承
朱兵
王保成
江浩
曹昕
卓厚天
张美君
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Nanjing Well Pharmaceutical Co ltd
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Nanjing Well Pharmaceutical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/006Refining fats or fatty oils by extraction
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/10Refining fats or fatty oils by adsorption

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

⑴ commercial industrial castor oil and an extracting agent are mixed and dissolved according to a certain proportion, ⑵ an adsorbent is added into the solution obtained in the step ⑴, stirring and adsorption are carried out, ⑶ filtration is carried out, the adsorbent is removed, ⑷ filtrate is cooled, standing and layering are carried out, the lower layer clear liquid is taken and the solvent is removed, and the castor oil finished product with low color and low acid value is obtained.

Description

Refining method of castor oil with low acid value and low chroma
Technical Field
The invention relates to a refining method of castor oil with low acid value and low chroma.
Background
Castor oil is one of ten and four inedible oil crops in the world, and the main production places are brazil and india. Castor oil is the only commercial grease mainly containing hydroxy acid, is a very important chemical raw material, can be directly used as a medical raw material, and can also be used for synthetic resin, coating, paint, soap, a plasticizer, an emulsifier, a lubricant and the like. At present, more than 70 million tons of castor oil are needed every year all over the world, and the effect can not be replaced.
Castor oil is usually prepared by crushing castor seeds and then adopting a cold pressing method, so that crude oil of the castor oil contains more impurities such as free fatty acid, pigment and the like, so that the castor oil cannot be directly used as a medicine, and needs to be refined by alkali refining, water washing, decoloring and other steps. Although the chroma and acid value of the refined castor oil are reduced to some extent, and the castor oil meets the standard requirements of pharmacopoeia of various countries, with the development of medical technology, higher quality requirements are provided for medicinal castor oil and medicinal auxiliary materials (such as polyoxyethylene (35) castor oil, hydrogenated castor oil, derivatives and the like) prepared by taking the castor oil as a raw material, and the quality of the castor oil directly determines the color and acid value of downstream products, so that the use safety of the downstream products as medicinal products is influenced.
The patent with application number CN88104649.3 proposes a mode of scouring castor oil with sodium hydroxide alkali, and the mode of active carbon and decoloration soil adsorption decolors castor oil, does not make clear expression to the effect of castor oil deacidification and decoloration, and this technology adopts a large amount of boiling water to spray the washing, produces a large amount of waste water. The patent with application number CN200910259593.2 uses an inorganic ceramic membrane to filter and ultrafilter medicinal castor oil and then enters a decoloring tower for decoloring, but the process has higher requirements on equipment and higher production cost, and the deacidification and decoloring effects are not mentioned. The patent with the application number of CN200810157273.1 proposes that the castor oil is deacidified and decolored by active carbon and argil, the acid value of the product is up to 1.5mgKOH/g, the chroma is Y10, and the requirement of high-quality medicinal castor oil cannot be met. The patent with application number CN201410387882.1 adopts a solvent extraction mode to extract castor oil from crushed castor seeds, and then the castor oil is subjected to adsorption treatment, and the acid value of the product is as high as 2 mgKOH/g. The patent with application number CN201510877807.8 adopts column chromatography to refine castor oil, which can reduce acid value and chroma and is not good for production scale-up.
At present, no industrial refining process report which can stably control the acid value of the castor oil to be less than or equal to 0.5mgKOH/g and the chroma to be less than or equal to Y3 is available.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method for refining low-acid-value and low-chroma castor oil.
An object of the present invention is to provide a method for refining castor oil to obtain castor oil meeting pharmaceutical requirements. The method comprises the following steps:
⑴ mixing commercial industrial castor oil and extractant at a certain ratio;
⑵ adding adsorbent into the solution obtained in step ⑴, stirring and adsorbing;
⑶ filtering to remove the adsorbent;
⑷ and cooling the filtrate, standing for layering, taking the supernatant and removing the solvent to obtain the castor oil product with low chroma and low acid value.
In one embodiment of the present invention, the extractant includes, but is not limited to, any one of petroleum ether, n-hexane, n-heptane or a mixture thereof.
In one embodiment of the present invention, the addition ratio of the extracting agent is: castor oil (w): 1: 1-1: 8 of an extracting agent (w);
in one embodiment of the invention, the adsorbent is any one of activated carbon, bleaching earth, activated clay, diatomite, alumina and magnesia or a mixture thereof;
in one embodiment of the invention, the amount of the refining agent is 5-50% of the mass of the castor oil;
in one embodiment of the present invention, the adsorption conditions are: the adsorption temperature is 40-80 ℃, and the adsorption time is 1-8 hours;
in one embodiment of the invention, the filtrate is cooled, kept stand and layered, the temperature is 20-30 ℃, and the time is 6-8 hours;
in an embodiment of the invention, according to the refining steps ⑴ - ⑷, the acid value of the obtained finished castor oil is less than or equal to 0.5mgKOH/g, and the chroma can be reduced from Y8 to Y3.
The solvent used in the invention can be recycled, the process is simple, and the scale-up production is easy. The acid value of the finished castor oil obtained by the invention is less than or equal to 0.5mgKOH/g, and the chroma can be reduced from Y8 to below Y3.
Detailed Description
Example 1:
a method for refining castor oil by using a high-purity castor oil,
10kg of castor oil and 40kg of petroleum ether are put into a reaction kettle, the temperature is raised to 50 ℃, and the castor oil and the petroleum ether are stirred and dissolved.
After the dissolution, 0.75kg of activated clay and 0.25kg of activated carbon are added, the mixture is kept at 50 ℃ and stirred for adsorption for 4 hours, and then the adsorbent is removed by filtration.
Transferring the filtrate to a liquid separation kettle, cooling to 25 ℃, standing for 6h for layering, and separating the lower layer clear liquid.
And (3) carrying out vacuum concentration on the lower clear liquid at the temperature of 80-90 ℃ to obtain 9.0kg of refined castor oil, wherein the detected acid value is 0.22mgKOH/g, and the chroma is Y3.
Example 2:
10kg of castor oil and 40kg of n-heptane are put into a reaction kettle, heated to 60 ℃, and stirred to be dissolved.
After the dissolution, 1kg of alumina and 0.25kg of active carbon are added, the mixture is kept at 60 ℃ and stirred for 6 hours, and then the adsorbent is removed by filtration.
Transferring the filtrate to a liquid separation kettle, cooling to 25 ℃, standing for 8h for layering, and separating the lower layer clear liquid.
And (3) carrying out vacuum concentration on the lower clear liquid at the temperature of 80-90 ℃ to obtain 9.2kg of refined castor oil, wherein the detected acid value is 0.20mgKOH/g, and the chroma is Y2.
Example 3:
10kg of castor oil and 40kg of normal hexane are added into a reaction kettle, and the temperature is raised to 55 ℃ to be stirred and dissolved.
After dissolution, 1kg of diatomite and 0.3kg of active carbon are added, the mixture is kept at 55 ℃ and stirred for adsorption for 5 hours, and then the adsorbent is removed by filtration.
Transferring the filtrate to a glass liquid separation kettle, cooling to 25 ℃, standing for 6 hours, and separating and taking the lower layer clear liquid.
And (3) concentrating the lower clear liquid in vacuum at 80-90 ℃ to obtain 8.9kg of refined castor oil, wherein the detected acid value is 0.24mgKOK/g, and the chroma is Y2.
Example 4:
10kg of castor oil and 40kg of normal hexane are added into a reaction kettle, and the temperature is raised to 60 ℃ to be stirred and dissolved.
After dissolution, 1kg of magnesium oxide and 0.4kg of active carbon are added, the mixture is kept at 60 ℃ and stirred for adsorption for 6 hours, and then the adsorbent is removed by filtration.
Transferring the filtrate to a glass liquid separation kettle, cooling to 25 ℃, standing for 6 hours, and separating and taking the lower layer clear liquid.
And (3) concentrating the lower clear liquid in vacuum at 80-90 ℃ to obtain 8.9kg of refined castor oil, wherein the detected acid value is 0.18mgKOK/g, and the chroma is Y2.
Example 5:
essentially the same as in example 1, except that the adsorbent described in step ⑵ was changed to a bleaching soil.
Example 6:
basically the same as example 1, except that the extractant in step ⑴ is a mixture of petroleum ether, n-hexane and n-heptane, and the amount of the extractant is 1 time of the mass of the castor oil, the adsorbent in step ⑵ is discolored soil, the adsorbent in step ⑵ is activated carbon, discolored soil, activated clay, diatomite, alumina and magnesium oxide, wherein the amount of the activated carbon is 1% of the mass of the castor oil, the amount of the other adsorbents is 1% of the mass of the castor oil, the stirring adsorption in step ⑵ is carried out at 40 ℃ for 6 hours, and the standing delamination in step ⑷ is carried out at 20-30 ℃ for 6 hours.
Example 7:
the process is substantially the same as example 1, except that the amount of the extractant used in step ⑴ is 8 times the mass of the castor oil, the adsorbent used in step ⑵ comprises 10% of activated carbon, the amount of the other adsorbents comprises 50% of castor oil, the adsorbent used in step ⑵ is stirred and adsorbed at 80 ℃ for 1 hour, and the adsorbent used in step ⑷ is allowed to stand for layering at 30 ℃ for 8 hours.
Example 8:
essentially the same as example 1, except that the amount of the extractant used in step ⑴ was 3 times the mass of castor oil, the adsorbent described in step ⑵, in which activated carbon was used in an amount of 2% of the mass of castor oil, the amount of the other adsorbents was 5% of the mass of castor oil, the adsorption temperature was 50 ℃ and the adsorption time was 6 hours in the stirred adsorption described in step ⑵, and the temperature was 20 ℃ and the time was 8 hours in the standing stratification described in step ⑷.
Example 9:
the method is basically the same as example 1, but the dosage of the extracting agent in step ⑴ is 6 times of the mass of the castor oil, wherein the dosage of the activated carbon is 4 percent of the mass of the castor oil, the dosage of the other adsorbing agents is 10 percent of the mass of the castor oil, the stirring adsorption in step ⑵ is carried out, the adsorption temperature is 60 ℃, the adsorption time is 4 hours, and the standing delamination in step ⑷ is carried out, the temperature is 30 ℃, and the time is 6 hours.

Claims (10)

1. A refining method of castor oil with low acid value and low chroma is characterized by comprising the following steps:
⑴ mixing commercial industrial castor oil and extractant at a certain ratio;
⑵ adding adsorbent into the solution obtained in step ⑴, stirring and adsorbing;
⑶ filtering to remove the adsorbent;
⑷ and cooling the filtrate, standing for layering, taking the supernatant and removing the solvent to obtain the castor oil product with low chroma and low acid value.
2. The method of claim 1, wherein said extraction agent of step ⑴ includes but is not limited to any one of petroleum ether, n-hexane, n-heptane or their mixture.
3. The method for refining castor oil with low acid value and low color number according to claim 1, wherein the amount of the extractant used in step ⑴ is 1-8 times of the mass of castor oil.
4. The method of claim 3, wherein the amount of the extractant used in step ⑴ is 4 times the mass of the castor oil.
5. The method of claim 1, wherein the adsorbent used in step ⑵ is selected from the group consisting of activated carbon, bleaching earth, activated clay, diatomaceous earth, alumina, and magnesia, or a mixture thereof.
6. The method for refining the castor oil with the low acid value and the low color number according to claim 1, wherein the adsorbent in step ⑵ comprises 1-10% by mass of activated carbon and 1-50% by mass of other adsorbents.
7. The method for refining the castor oil with the low acid value and the low color number according to claim 6, wherein the adsorbent in step ⑵ comprises 2-4% by mass of activated carbon and 5-10% by mass of other adsorbents.
8. The method for refining the castor oil with the low acid value and the low color number according to claim 1, wherein the stirring and the adsorption are performed at the temperature of 40 to 80 ℃ for 1 to 8 hours in step ⑵.
9. The refining method of castor oil with low acid value and low chroma according to claim 8, wherein the stirring and adsorption of step ⑵ are carried out at 50-60 ℃ for 4-6 hours.
10. The method for refining the castor oil with the low acid value and the low color number according to any one of claims 1 to 9, wherein the standing for layering in the step ⑷ is performed at a temperature of 20 to 30 ℃ for 6 to 8 hours.
CN201911250436.5A 2019-12-09 2019-12-09 Refining method of castor oil with low acid value and low chroma Pending CN111234920A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114874849A (en) * 2022-05-30 2022-08-09 南京威尔药业科技有限公司 Method for refining castor oil with low chroma and low acid value

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1486795A (en) * 1974-09-24 1977-09-21 Nisshin Oil Mills Ltd Method of refining palm oil
CN101311250A (en) * 2007-05-25 2008-11-26 北京化工大学 Novel diesel fuel decolorant and decolouring process
CN101709245A (en) * 2009-12-21 2010-05-19 湖南尔康制药有限公司 Method for refining medicinal castor oil
CN102517148A (en) * 2011-12-20 2012-06-27 山东渤海实业股份有限公司 Two-step decolorization method for phospholipid
CN103013653A (en) * 2012-12-28 2013-04-03 广州白云山汉方现代药业有限公司 Preparation method of refined egg oil
CN103087820A (en) * 2012-07-11 2013-05-08 哈尔滨商业大学 Process method for reducing color and luster of soybean oil by two-section type de-coloring
CN103305339A (en) * 2013-06-24 2013-09-18 内蒙古天润蓖麻开发有限公司 Dehydration and decoloration low-emission production process of refined castor oil

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1486795A (en) * 1974-09-24 1977-09-21 Nisshin Oil Mills Ltd Method of refining palm oil
CN101311250A (en) * 2007-05-25 2008-11-26 北京化工大学 Novel diesel fuel decolorant and decolouring process
CN101709245A (en) * 2009-12-21 2010-05-19 湖南尔康制药有限公司 Method for refining medicinal castor oil
CN102517148A (en) * 2011-12-20 2012-06-27 山东渤海实业股份有限公司 Two-step decolorization method for phospholipid
CN103087820A (en) * 2012-07-11 2013-05-08 哈尔滨商业大学 Process method for reducing color and luster of soybean oil by two-section type de-coloring
CN103013653A (en) * 2012-12-28 2013-04-03 广州白云山汉方现代药业有限公司 Preparation method of refined egg oil
CN103305339A (en) * 2013-06-24 2013-09-18 内蒙古天润蓖麻开发有限公司 Dehydration and decoloration low-emission production process of refined castor oil

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114874849A (en) * 2022-05-30 2022-08-09 南京威尔药业科技有限公司 Method for refining castor oil with low chroma and low acid value

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