CN110257169A - A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content - Google Patents

A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content Download PDF

Info

Publication number
CN110257169A
CN110257169A CN201910507376.4A CN201910507376A CN110257169A CN 110257169 A CN110257169 A CN 110257169A CN 201910507376 A CN201910507376 A CN 201910507376A CN 110257169 A CN110257169 A CN 110257169A
Authority
CN
China
Prior art keywords
low
palm oil
ester
grease
content
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910507376.4A
Other languages
Chinese (zh)
Inventor
刘志
刘欢
黄艺强
袁向华
谢黔岭
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenzhen Jingyi Oil & Fat Technology Co Ltd
Original Assignee
Shenzhen Jingyi Oil & Fat Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenzhen Jingyi Oil & Fat Technology Co Ltd filed Critical Shenzhen Jingyi Oil & Fat Technology Co Ltd
Priority to CN201910507376.4A priority Critical patent/CN110257169A/en
Publication of CN110257169A publication Critical patent/CN110257169A/en
Pending legal-status Critical Current

Links

Classifications

    • 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

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Chemical & Material Sciences (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)
  • Lubricants (AREA)

Abstract

The present invention relates to the refining manufacture field of palm oil, a kind of method for further relating to palm oil for preparing low ethylene oxidic ester and low 3-MCPD ester content, including following preparation step: degumming process A, is carried out to palm oil;B, solvent point is carried out to the palm oil after the step A degumming process to mention, then carry out deodorization processing, obtain the grease of low diglyceride content;C, the palm oil of low ethylene oxidic ester and low 3-MCPD ester content is made into shape refining treatment to the grease of the low diglyceride content of the step B, and effectively reduces refining difficulty, reduce refining cost.

Description

A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content
Technical field
The present invention relates to the refining manufacture field of palm oil, a kind of low ethylene oxidic ester and low of preparing is further related to The method of the palm oil of 3-MCPD ester content.
Background technique
Glycidol is a kind of with gene tumorigenic compound, is condensed and is formed through 1,2 hydroxyls dehydrate by glycerol.IARC (International Agency for Research on Cancer), glycidol is classified as by international cancer research institution 2A class carcinogenic substance mainly exists in grease in the form of glycidol aliphatic ester (abbreviation ethylene oxidic ester), wherein shrinking Glyceryl oleate and glycidol stearate are classified as 3 class carcinogenic substances by IARC.The epoxy based structures of glycidol have very strong Reactivity be easily converted into chloropropyl alcohol such as in the presence of hydrochloric acid, ethylene oxidic ester is metabolizable in vivo to endanger for glycidol Evil human health.
The chloro- 1,2- propylene glycol (3-MCPD) of 3- has Toxicity of Kidney, genotoxicity, neurotoxicity, immunotoxicity, mutagenesis Property and carcinogenicity, IARC are classified as 2B class carcinogenic substance.Mainly with 3-MCPD aliphatic ester (abbreviation 3-MCPD ester) in grease Form exist, 3-MCPD ester is metabolized as 3-MCPD and endangers health through hydrolysis in vivo other than the toxicity of itself.
Researchers at home and abroad detect 3- in the food from numerous food such as animal and plant fat and containing animal and plant fat MCPD ester and ethylene oxidic ester draw especially in baby milk powder after the 3-MCPD ester and ethylene oxidic ester of discovery high concentration Play the great attention of government and oil prodution industry.And refined palm oil is one of large glyceride stock, is answered extensively in the food industry With, however it has the risk of high ethylene oxidic ester and high 3-MCPD ester content level, keeps the use of palm oil strong for human body Health is there are certain harm, using having some limitations.
Summary of the invention
For overcome the deficiencies in the prior art, the present invention, which provides, a kind of prepares low ethylene oxidic ester and low 3-MCPD ester content Palm oil method, this method is easy to operate, and condition is controllable, and the content of the ethylene oxidic ester in palm oil obtained is in 1ppm Hereinafter, the content of 3-MCPD ester is in 3ppm or less.
The technical solution adopted by the present invention to solve the technical problems is:
A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content comprising following preparation step It is rapid:
A, degumming process is carried out to palm oil;
B, solvent point is carried out to the palm oil after the step A degumming process to mention, then carry out deodorization processing, obtain low sweet The grease of two ester contents;
C, refining treatment is carried out to the grease of the low diglyceride content of the step B, low ethylene oxidic ester and low 3- is made The palm oil of MCPD ester content.
Palm oil contains the diglyceride of higher level, and diglyceride is the major prerequisites object of ethylene oxidic ester and 3-MCPD ester Matter, the present invention reduces the diglyceride content in palm oil by using the mode that solvent point mentions, then again to low diglyceride content Grease further progress refining treatment, the ethylene oxidic ester of treated palm oil and the content of 3-MCPD ester are extremely low.
Wherein, the refining treatment in the step C is refined using common process condition, easy to operate, is advantageously reduced into This, improves production efficiency.
Wherein, the solvent in the step B point, which mentions, includes the following steps:
(1) by after the step A degumming process palm oil and solvent under conditions of 40-60 DEG C be uniformly mixed, so Mixture is cooled down step by step afterwards, cooling and stirring to fat crystals is completed;
(2) grease and solvent mixture are separated by solid-liquid separation, and to after separation solid and liquid carry out precipitation respectively, be made The grease of low diglyceride content.
Wherein, it is described step by step cooling, cooling and stirring operating condition are as follows: it is described step by step cooling, cooling and stirring operation item Part are as follows: cooling down is carried out to mixture under conditions of temperature is 25-35 DEG C, mixing speed is 35-45rpm, it is described A length of 1-2h when the stirring of cooling down;To mixing under conditions of temperature is 18-22 DEG C, mixing speed is 35-45rpm Object is cooled down twice cooling, when reducing temperature twice cooling stirring a length of 1-3h;Temperature is 5-15 DEG C, mixing speed is Cooling down three times carried out to mixture under conditions of 35-45rpm, when stirring of the cooling down three times a length of 3-16h.
Wherein, the solvent is at least one of n-hexane, acetone, ethyl alcohol.
Wherein, the volume of the solvent is 1-2.5 times of the palm oil volume after the step A degumming process.
Wherein, the diglyceride content in the grease of the low diglyceride content is less than 3%.
Preferably, the diglyceride content in the grease of the low diglyceride content is less than 2%.
It is highly preferred that the diglyceride content in the grease of the low diglyceride content is less than 1.6%.
Wherein, it carries out multiple solvent point to the palm oil after the step A degumming process to mention, to meet lower diglyceride Content requirement, or obtain more low diglyceride content greases.
The beneficial effects of the present invention are:
1, palm oil obtains the grease of low diglyceride content after solvent point mentions, and further low 3- can be obtained in refining The palm oil grease of MCPD ester and low ethylene oxidic ester, wherein the content of ethylene oxidic ester is in 1ppm hereinafter, 3-MCPD ester contains Amount is in 3ppm or less.Relative to the grease mentioned without solvent point, the harsh refining of condition need to be passed through, can just obtain low 3-MCPD Refining difficulty is effectively reduced in the palm oil of ester and low ethylene oxidic ester, the present invention, reduces refining cost;
2, solvent used can recycle and reuse when solvent point mentions, and reduce the pollution to environment.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is in the embodiment of the present invention 1 without a point HPLC-ELSD chromatogram for the palm oil mentioned;
Fig. 2 is the grease HPLC-ELSD chromatogram in the supernatant liquid of present example 6;
Fig. 3 is the grease HPLC-ELSD chromatogram in 6 lower liquid of present example;
Fig. 4 is that present example 6 divides and mentions obtained solid grease HPLC-ELSD chromatogram.
Specific embodiment
For the ease of the understanding of those skilled in the art, the present invention is made into one below with reference to embodiment, table and attached drawing The explanation of step, the content that embodiment refers to not are limitation of the invention.
Embodiment 1
A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content comprising following preparation step It is rapid:
A, degumming process is carried out to palm oil;
B, solvent point is carried out to the palm oil after the step A degumming process to mention, then carry out deodorization processing, obtain low sweet The grease of two ester contents;
C, low ethylene oxidic ester and low 3- are made into shape refining treatment to the grease of the low diglyceride content of the step B The palm oil of MCPD ester content.
Wherein, the degumming process and deodorization processing are existing common process, are not gone to live in the household of one's in-laws on getting married herein to its specific steps It states.Refining treatment in the step C is refined using common process condition, is not repeated herein its specific steps.
Wherein, the solvent in the step B point, which mentions, includes the following steps:
(1) it is stirred in the temperature control formed with the new sesame DCW-1015 type water-bath in Ningbo with Changsha day wound JM-3 type agitating ball mill It mixes in system, by palm oil of the 100mL after the step A degumming process and 200mL n-hexane solvent under conditions of 50 DEG C It is uniformly mixed, then mixture is cooled down step by step, cooling and stirring to fat crystals is completed;The cooling step by step, cooling are stirred The operating condition mixed are as follows: first once cooled down under conditions of temperature is 30 DEG C, mixing speed is 40rpm to mixture cold But, a length of 1.5h when the stirring of a cooling down;Then under conditions of temperature is 20 DEG C, mixing speed is 40rpm Cooling is cooled down twice to mixture, when reducing temperature twice cooling stirring a length of 2.5h;Further temperature be 10 DEG C, Mixing speed carries out cooling down three times to mixture under conditions of being 40rpm, and when stirring of the cooling down three times is a length of 16h completes fat crystals.
(2) after cooling and stirring, rapidly to Tian Jinjin rise GM-0.33 diaphragm-type vacuum pump and sand core suction funnel and Boiling flask forms in suction filtration system, and grease and solvent mixture, which filter, makes separation of solid and liquid obtain liquid and solid, and To after separation liquid and solid carry out precipitation, liquid portion directly rises GM-0.33 diaphragm-type vacuum pump, Germany to Tian Jinjin Solvent recovery/desolventizing system of IKA C-MAG HS-7 type digital display heating plate, condenser pipe and boiling flask composition carries out precipitation.It takes out Filter funnel be cleaned multiple times with n-hexane solvent after, by cleaning solution and filter obtained solid grease be placed in it is same newly it is flat Precipitation is carried out in flask, and the grease of low diglyceride content is made.
Diglyceride content in the grease of the low diglyceride content is 1.69%.
Embodiment 2
A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content comprising following preparation step It is rapid:
A, degumming process is carried out to palm oil;
B, solvent point is carried out to the palm oil after the step A degumming process to mention, then carry out deodorization processing, obtain low sweet The grease of two ester contents;
C, low ethylene oxidic ester and low 3- are made into shape refining treatment to the grease of the low diglyceride content of the step B The palm oil of MCPD ester content.
Wherein, the degumming process and deodorization processing are existing common process, are not gone to live in the household of one's in-laws on getting married herein to its specific steps It states.Refining treatment in the step C is refined using common process condition, is not repeated herein its specific steps.
Wherein, the solvent in the step B point, which mentions, includes the following steps:
(1) it is stirred in the temperature control formed with the new sesame DCW-1015 type water-bath in Ningbo with Changsha day wound JM-3 type agitating ball mill It mixes in system, by palm oil of the 200mL after the step A degumming process and 200mL n-hexane solvent under conditions of 50 DEG C It is uniformly mixed, then mixture is cooled down step by step, cooling and stirring to fat crystals is completed;The cooling step by step, cooling are stirred The operating condition mixed are as follows: first once cooled down under conditions of temperature is 30 DEG C, mixing speed is 40rpm to mixture cold But, a length of 1h when the stirring of a cooling down;Then right under conditions of temperature is 20 DEG C, mixing speed is 40rpm Mixture is cooled down twice cooling, when reducing temperature twice cooling stirring a length of 1h;Further it is 15 DEG C, stirs in temperature Speed carries out cooling down three times to mixture under conditions of being 40rpm, when stirring of the cooling down three times a length of 3h, make Fat crystals are completed.
(2) after cooling and stirring, rapidly to Tian Jinjin rise GM-0.33 diaphragm-type vacuum pump and sand core suction funnel and Boiling flask forms in suction filtration system, and grease and solvent mixture, which filter, makes separation of solid and liquid obtain liquid and solid, and To after separation liquid and solid carry out precipitation, liquid portion directly rises GM-0.33 diaphragm-type vacuum pump, Germany to Tian Jinjin Solvent recovery/desolventizing system of IKA C-MAG HS-7 type digital display heating plate, condenser pipe and boiling flask composition carries out precipitation, takes out Filter funnel be cleaned multiple times with n-hexane solvent after, by cleaning solution and filter obtained solid grease be placed in it is same newly it is flat Precipitation is carried out in flask, and the grease of low diglyceride content is made.
Diglyceride content in the grease of the low diglyceride content is 2.31%.
Embodiment 3
A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content, embodiment 3 and embodiment 2 Difference is, carry out in stepb palm oil when solvent point mentions using 150mL after the step A degumming process with by The mixed solvent of 125mL n-hexane and 75mL dehydrated alcohol composition is mixed, the other operating procedures and operation item of embodiment 3 Part is same as Example 2, and this will not be repeated here.
Diglyceride content in the grease of the low diglyceride content is 1.96%.
Embodiment 4
A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content, embodiment 4 and embodiment 2 Difference is, carry out in stepb palm oil when solvent point mentions using 210mL after the step A degumming process with by 140mL n-hexane and 70mL acetone composition mixed solvent mixed, the other operating procedures and operating condition of embodiment 4 with Embodiment 2 is identical, and this will not be repeated here.
Diglyceride content in the grease of the low diglyceride content is 2.37%.
Embodiment 5
A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content, embodiment 4 and embodiment 2 Difference is, carries out the palm oil and 250mL when solvent point mentions using 200mL after the step A degumming process in stepb Acetone solvent is mixed, and the other operating procedures and operating condition of embodiment 5 are same as Example 2, and this will not be repeated here.
Diglyceride content in the grease of the low diglyceride content is 2.04%.
Embodiment 6
A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content comprising following preparation step It is rapid:
A, degumming process is carried out to palm oil;
B, solvent point is carried out to the palm oil after the step A degumming process to mention, then carry out deodorization processing, obtain low sweet The grease of two ester contents;
C, low ethylene oxidic ester and low 3- are made into shape refining treatment to the grease of the low diglyceride content of the step B The palm oil of MCPD ester content.
Wherein, the degumming process and deodorization processing are existing common process, are not gone to live in the household of one's in-laws on getting married herein to its specific steps It states.Refining treatment in the step C is refined using common process condition, is not repeated herein its specific steps.
Wherein, the solvent in the step B point, which mentions, includes the following steps:
(1) it is stirred in the temperature control formed with the new sesame DCW-1015 type water-bath in Ningbo with Changsha day wound JM-3 type agitating ball mill It mixes in system, by palm oil of the 200mL after the step A degumming process and by 100mL n-hexane and 400mL dehydrated alcohol group At mixed solvent mixing, and under conditions of 50 DEG C be uniformly mixed, then mixture is cooled down step by step, cooling and stirring extremely Fat crystals are completed;It is described step by step cooling, cooling and stirring operating condition are as follows: first temperature be 30 DEG C, mixing speed 40rpm Under conditions of a cooling down carried out to mixture, when stirring of a cooling down a length of 1h;Then it is in temperature 20 DEG C, mixing speed cooling is cooled down twice to mixture under conditions of being 40rpm, when the cooling stirring of the reducing temperature twice A length of 1h;Cooling down three times, institute further are carried out to mixture under conditions of temperature is 15 DEG C, mixing speed is 40rpm A length of 3h when the stirring of cooling down three times is stated, fat crystals are completed.
(2) after cooling and stirring, rapidly to Tian Jinjin rise GM-0.33 diaphragm-type vacuum pump and sand core suction funnel and Boiling flask forms in suction filtration system, and grease and solvent mixture, which filter, makes separation of solid and liquid obtain liquid and solid, institute The liquid portion obtained divides upper layer and lower layer, is first separated with liquid of the separatory funnel to upper and lower level, then to the upper and lower level after separation Liquid and solid grease carry out precipitation respectively, and GM-0.33 diaphragm-type vacuum pump, moral are directly risen to Tian Jinjin in liquid solvent part Solvent recovery/desolventizing system of state IKA C-MAG HS-7 type digital display heating plate, condenser pipe and boiling flask composition carries out precipitation. After suction funnel is cleaned multiple times with the mixed solvent being made of n-hexane and dehydrated alcohol, by cleaning solution and gained is filtered admittedly Body grease is placed in the same new boiling flask and carries out precipitation, and the grease of low diglyceride content is made.
Diglyceride content in the grease of the low diglyceride content is 1.56%.
Embodiment 7
A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content comprising following preparation step It is rapid:
A, degumming process is carried out to palm oil;
B, solvent point is carried out to the palm oil after the step A degumming process to mention, then carry out deodorization processing, obtain low sweet The grease of two ester contents;
C, low ethylene oxidic ester and low 3- are made into shape refining treatment to the grease of the low diglyceride content of the step B The palm oil of MCPD ester content.
Wherein, the degumming process and deodorization processing are existing common process, are not gone to live in the household of one's in-laws on getting married herein to its specific steps It states.Refining treatment in the step C is refined using common process condition, is not repeated herein its specific steps.
Wherein, the solvent in the step B point, which mentions, includes the following steps:
(1) it is stirred in the temperature control formed with the new sesame DCW-1015 type water-bath in Ningbo with Changsha day wound JM-3 type agitating ball mill It mixes in system, by palm oil of the 100mL after the step A degumming process and 200mL n-hexane solvent under conditions of 50 DEG C It is uniformly mixed, then mixture is cooled down step by step, cooling and stirring to fat crystals is completed;The cooling step by step, cooling are stirred The operating condition mixed are as follows: first once cooled down under conditions of temperature is 25 DEG C, mixing speed is 35rpm to mixture cold But, a length of 1h when the stirring of a cooling down;Then right under conditions of temperature is 18 DEG C, mixing speed is 35rpm Mixture is cooled down twice cooling, when reducing temperature twice cooling stirring a length of 1h;Further it is 5 DEG C, stirs in temperature Speed carries out cooling down three times to mixture under conditions of being 35rpm, when stirring of the cooling down three times a length of 3h, make Fat crystals are completed.
(2) after cooling and stirring, rapidly to Tian Jinjin rise GM-0.33 diaphragm-type vacuum pump and sand core suction funnel and Boiling flask forms in suction filtration system, and grease and solvent mixture, which filter, makes separation of solid and liquid obtain liquid and solid, and To after separation liquid and solid carry out precipitation, liquid solvent part directly to Tian Jinjin rise GM-0.33 diaphragm-type vacuum pump, Solvent recovery/desolventizing system of German IKA C-MAG HS-7 type digital display heating plate, condenser pipe and boiling flask composition is taken off It is molten.After suction funnel is cleaned multiple times with n-hexane solvent, cleaning solution and suction filtration obtained solid grease are placed in same new Boiling flask in carry out precipitation, the grease of low diglyceride content is made.
Diglyceride content in the grease of the low diglyceride content is 2.35%.
Embodiment 8
A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content comprising following preparation step It is rapid:
A, degumming process is carried out to palm oil;
B, solvent point is carried out to the palm oil after the step A degumming process to mention, then carry out deodorization processing, obtain low sweet The grease of two ester contents;
C, low ethylene oxidic ester and low 3- are made into shape refining treatment to the grease of the low diglyceride content of the step B The palm oil of MCPD ester content.
Wherein, the degumming process and deodorization processing are existing common process, are not gone to live in the household of one's in-laws on getting married herein to its specific steps It states.Refining treatment in the step C is refined using common process condition, is not repeated herein its specific steps.
Wherein, the solvent in the step B point, which mentions, includes the following steps:
(1) it is stirred in the temperature control formed with the new sesame DCW-1015 type water-bath in Ningbo with Changsha day wound JM-3 type agitating ball mill It mixes in system, by palm oil of the 100mL after the step A degumming process and 200mL n-hexane solvent under conditions of 50 DEG C It is uniformly mixed, then mixture is cooled down step by step, cooling and stirring to fat crystals is completed;The cooling step by step, cooling are stirred The operating condition mixed are as follows: first once cooled down under conditions of temperature is 35 DEG C, mixing speed is 45rpm to mixture cold But, a length of 2h when the stirring of a cooling down;Then right under conditions of temperature is 22 DEG C, mixing speed is 45rpm Mixture is cooled down twice cooling, when reducing temperature twice cooling stirring a length of 3h;Further it is 15 DEG C, stirs in temperature Speed carries out cooling down three times to mixture under conditions of being 45rpm, when stirring of the cooling down three times a length of 9.5h, Complete fat crystals.
(2) after cooling and stirring, rapidly to Tian Jinjin rise GM-0.33 diaphragm-type vacuum pump and sand core suction funnel and Boiling flask forms in suction filtration system, and grease and solvent mixture, which filter, makes separation of solid and liquid obtain liquid and solid, and To after separation liquid and solid carry out precipitation, liquid portion directly rises GM-0.33 diaphragm-type vacuum pump, Germany to Tian Jinjin Solvent recovery/desolventizing system of IKAC-MAG HS-7 type digital display heating plate, condenser pipe and boiling flask composition carries out precipitation.It takes out Filter funnel be cleaned multiple times with n-hexane solvent after, by cleaning solution and filter obtained solid grease be placed in it is same newly it is flat Precipitation is carried out in flask.
(3) step (1) and step (2) are repeated, the grease of low diglyceride content is made.
Diglyceride content in the grease of the low diglyceride content is 1.20%.
Testing inspection: diglyceride is detected to the grease HPLC-ELSD method of the low diglyceride content after embodiment 1-6 precipitation Content (using area percentage as content), and the result after will test is recorded in table 1, and do not divide the HPLC- for mentioning palm oil ELSD chromatogram such as Fig. 1, grease HPLC-ELSD chromatogram such as Fig. 2 in 6 supernatant liquid of example, the oil in 6 lower liquid of example Rouge HPLC-ELSD chromatogram such as Fig. 3, example 6 divide that mention obtained solid grease HPLC-ELSD chromatogram as shown in Figure 4.
Diglyceride detection method of content is as follows: liquid chromatograph-HPLC1500, American science system;ELSD— ELSD2000ES, the U.S. are difficult to understand safe;Chromatographic column -5 μ 50mm × 4.6mm of Alltima TM C18 × 5um, the U.S. are difficult to understand safe;Column temperature- 42℃;Mobile phase-acetonitrile: n-hexane: isopropanol=270:80:100v/v/v;Flow velocity -1mL/min;Runing time- 45min;ELSD condition: 80 DEG C, 2mL/min.
Diglyceride content in the grease of the low diglyceride content of 1 embodiment 1-6 of table
As shown in Table 1, diglyceride content exists in the grease of low diglyceride content made from preparation method of the invention Between 1.20%-2.37%, then to the grease further progress refining treatment of low diglyceride content, through detecting, it is brown that treated The ethylene oxidic ester of palmitic acid oil and the content of 3-MCPD ester are extremely low, and wherein the content of ethylene oxidic ester is in 1ppm hereinafter, 3-MCPD ester Content in 3ppm or less.
It is to be illustrated to preferable implementation of the invention, but the invention is not limited to the implementation above Example, those skilled in the art can also make various equivalent variations on the premise of without prejudice to spirit of the invention or replace It changes, these equivalent deformations or replacement are all included in the scope defined by the claims of the present application.

Claims (6)

1. a kind of method for the palm oil for preparing low ethylene oxidic ester and low 3-MCPD ester content, it is characterised in that: including as follows Preparation step:
A, degumming process is carried out to palm oil;
B, solvent point is carried out to the palm oil after the step A degumming process to mention, then carry out deodorization processing, obtain low diglyceride The grease of content;
C, low ethylene oxidic ester and low 3-MCPD are made into shape refining treatment to the grease of the low diglyceride content of the step B The palm oil of ester content.
2. a kind of method of palm oil for preparing low ethylene oxidic ester and low 3-MCPD ester content according to claim 1, It is characterized by: the solvent point in the step B mentions and including the following steps:
(1) by after the step A degumming process palm oil and solvent under conditions of 40-60 DEG C be uniformly mixed, then will Mixture is cooled down step by step, cooling and stirring to fat crystals is completed;
(2) grease and solvent mixture are separated by solid-liquid separation, and to after separation solid and liquid carry out precipitation respectively, be made low sweet The grease of two ester contents.
3. a kind of method of palm oil for preparing low ethylene oxidic ester and low 3-MCPD ester content according to claim 2, It is characterized by: the operating condition of cooling step by step, cooling and stirring in the step (1) are as follows: be 25-35 DEG C, stir in temperature Speed carries out a cooling down to mixture under conditions of being 35-45rpm, when stirring of a cooling down a length of 1- 2h;Cooling is cooled down twice to mixture under conditions of temperature is 18-22 DEG C, mixing speed is 35-45rpm, described two A length of 1-3h when the stirring of secondary cooling down;To mixture under conditions of temperature is 5-15 DEG C, mixing speed is 35-45rpm Carry out cooling down three times, when stirring of the cooling down three times a length of 3-16h.
4. a kind of method of palm oil for preparing low ethylene oxidic ester and low 3-MCPD ester content according to claim 2, It is characterized by: the solvent in the step (1) is at least one of n-hexane, acetone, ethyl alcohol.
5. a kind of method of palm oil for preparing low ethylene oxidic ester and low 3-MCPD ester content according to claim 2, It is characterized by: the volume of the solvent in the step (1) is the 1- of the palm oil volume after the step A degumming process 2.5 again.
6. a kind of method of palm oil for preparing low ethylene oxidic ester and low 3-MCPD ester content according to claim 1, It is characterized by: the diglyceride content in the grease of the low diglyceride content is less than 3%.
CN201910507376.4A 2019-06-12 2019-06-12 A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content Pending CN110257169A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910507376.4A CN110257169A (en) 2019-06-12 2019-06-12 A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910507376.4A CN110257169A (en) 2019-06-12 2019-06-12 A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content

Publications (1)

Publication Number Publication Date
CN110257169A true CN110257169A (en) 2019-09-20

Family

ID=67917890

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910507376.4A Pending CN110257169A (en) 2019-06-12 2019-06-12 A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content

Country Status (1)

Country Link
CN (1) CN110257169A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111233813A (en) * 2020-03-05 2020-06-05 浙江伊宝馨生物科技股份有限公司 Method for removing glycidyl ester in mixed tocopherol

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB8615625D0 (en) * 1985-07-01 1986-07-30 Fuji Oil Co Ltd Fractionation of fats & oils
WO2011002275A1 (en) * 2009-06-30 2011-01-06 Sime Darby Malaysia Berhad Process for manufacturing palm oil fractions containing virtually no 3-monochloropropanediol fatty acid esters
WO2013163112A1 (en) * 2012-04-27 2013-10-31 Archer Daniels Midland Company Improved fractionation processes
CN104629906A (en) * 2013-11-07 2015-05-20 丰益(上海)生物技术研发中心有限公司 Crystallization aid and fat fractionation method
CN105602720A (en) * 2016-03-22 2016-05-25 江南大学 Method for fractionating mango kernel fat by virtue of solvent
WO2016089196A1 (en) * 2014-12-03 2016-06-09 Sime Darby Malaysia Berhad Continuous process for dry fractionation of glyceride oils
WO2019103667A1 (en) * 2017-11-22 2019-05-31 Aak Ab (Publ) Process for dry fractionation of a palm oil olein

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB8615625D0 (en) * 1985-07-01 1986-07-30 Fuji Oil Co Ltd Fractionation of fats & oils
WO2011002275A1 (en) * 2009-06-30 2011-01-06 Sime Darby Malaysia Berhad Process for manufacturing palm oil fractions containing virtually no 3-monochloropropanediol fatty acid esters
WO2013163112A1 (en) * 2012-04-27 2013-10-31 Archer Daniels Midland Company Improved fractionation processes
CN104629906A (en) * 2013-11-07 2015-05-20 丰益(上海)生物技术研发中心有限公司 Crystallization aid and fat fractionation method
WO2016089196A1 (en) * 2014-12-03 2016-06-09 Sime Darby Malaysia Berhad Continuous process for dry fractionation of glyceride oils
CN105602720A (en) * 2016-03-22 2016-05-25 江南大学 Method for fractionating mango kernel fat by virtue of solvent
WO2019103667A1 (en) * 2017-11-22 2019-05-31 Aak Ab (Publ) Process for dry fractionation of a palm oil olein

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
俞良莉等: "《食品安全化学》", 31 October 2014, 上海交通大学出版社 *
马传国: "《油脂深加工与制品》", 30 September 2022, 中国商业出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111233813A (en) * 2020-03-05 2020-06-05 浙江伊宝馨生物科技股份有限公司 Method for removing glycidyl ester in mixed tocopherol

Similar Documents

Publication Publication Date Title
EP2611767B1 (en) Elimination of organohalo and oxirane species in carboxylic acid ester streams
CN110257169A (en) A method of preparing the palm oil of low ethylene oxidic ester and low 3-MCPD ester content
WO2014071736A1 (en) Method for extracting silkworm pupa oil
CN208414360U (en) A kind of essential oil extraction device
CN107057858A (en) Reduce the supercritical carbon dioxide method for extracting and device of extract acid value
CN100567368C (en) From glycerol slag, extract the method for Polyglycerine
CN102618383B (en) Production method and system of deacidification rice bran oil
CN103937616B (en) Method for extracting high-purity unsaturated fatty acid from soybean oil
CN106565662B (en) Macrocyclic musk-pentadacanolide method is prepared using Malania Oleifera Oil
CN102070411B (en) Method for refining honokiol
CN109666533A (en) Refined horse oil and its refining extracting method and application
CN208372529U (en) A kind of producing base oil by regenerating waste lubricating oil solvent extraction system
CN110791376B (en) Supercritical CO 2 Method for removing free fatty acid in camellia seed oil by microemulsion
CN104292198B (en) During maltol produces, grignard is hydrolyzed two-phase laminated flow synthetic method and device
CN105062658B (en) A kind of green extraction process of lacquer tree fat
CN202270376U (en) Continuous rectifying device
CN106220527A (en) A kind of DMF rectifying and dewatering method of purification
CN108676624A (en) The extracting method and Rosa Damascana of Rosa Damascana
CN109439426A (en) A kind of arrow-leaved oleaster oil and preparation method thereof and purposes as biodiesel raw material
JP2016185998A (en) Manufacturing method of refined palm oil with reduced content of monochloro propanediol product
CN104447244A (en) Roflumilast intermediates and preparation method of roflumilast
JP6405220B2 (en) Method for producing refined fats and oils
CN105104583B (en) The preparation method of middle long-chain fat acid lipid
CN108084016A (en) A kind of high-purity linoleic preparation method
CN113234525A (en) Method for producing yellow mealworm oil at low temperature

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190920