CN102876452A - Soybean oil degumming method utilizing alkali refining waste water treated by inorganic ceramic membrane - Google Patents

Soybean oil degumming method utilizing alkali refining waste water treated by inorganic ceramic membrane Download PDF

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Publication number
CN102876452A
CN102876452A CN2012103785476A CN201210378547A CN102876452A CN 102876452 A CN102876452 A CN 102876452A CN 2012103785476 A CN2012103785476 A CN 2012103785476A CN 201210378547 A CN201210378547 A CN 201210378547A CN 102876452 A CN102876452 A CN 102876452A
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China
Prior art keywords
waste water
oil
ceramic membrane
washing waste
alkali refining
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CN2012103785476A
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Chinese (zh)
Inventor
王立琦
于殿宇
江连洲
胡立志
时敏
常云鹤
宋鹏
李万振
刘鑫
宋云花
张春艳
邹小雨
王玥
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Harbin University of Commerce
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Harbin University of Commerce
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Priority to CN2012103785476A priority Critical patent/CN102876452A/en
Publication of CN102876452A publication Critical patent/CN102876452A/en
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  • Fats And Perfumes (AREA)
  • Edible Oils And Fats (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The invention relates to a soybean oil degumming method utilizing alkali refining waste water treated by inorganic ceramic membrane. In the method, wastewater generated in edible oil processing is treated by the inorganic ceramic membrane technology, the treated wastewater is then applied to an oil degumming process, so that environmental pollution caused by the wastewater discharged directly is reduced while resources and energy are saved, industrial production cost is reduced to a great extent, and degumming effect of the method is better than that of other degumming methods. Since the wastewater with pH (potential of hydrogen) value equal to 7.5, the saponified matter content equal to 0.67% and the oil content equal to 9.1mg/L, generated after the ceramic membrane treatment, is applied to soybean oil degumming, the measured phosphorus content is about 5mg/kg; and on the condition of gauge pressure equal to 300kPa, steam consumption can be saved by 0.016 ton/per ton of oil for processing of soybean oil.

Description

A kind of method of coming unstuck for soybean oil with inorganic ceramic film processing alkali refining waste water
Technical field:
The present invention relates to a kind of of food oils manufacture field and process the method that alkali refining waste water comes unstuck for soybean oil with inorganic ceramic film.
Background technology:
The general employing of depickling is neutralization, washing process in oil and fat refining process, by using in the alkali and the free fatty acids in the grease, generate the centrifugation from oil of Chinese honey locust other impurity of absorbed portion, and then add water the excess alkali in the oil is washed, produce thus washes, be dissolved with the alkali of fatty acid sodium soap and excess etc. in these waste water, as directly entering the river, not only reduce dissolved oxygen in the water, cause water-quality deterioration, affect the existence of organism in water, but also affect agricultural irrigation and the resident drinks, cause environmental pollution.Adopt conventional materialization, Biochemical Treatment not good, and cost is high, waste oil can not reclaim after processing, and the wasting of resources is large.
Mineral membrane is high temperature resistant, acid and alkali-resistance and organic corrosion are a kind of Polar Crystal Slabs, has stronger hydrophilic oleophobic performance, and can in filtration procedure, form the layer of gel layer, thereby in actual filtration, often can hold back than membrane pore size little oil droplet far away, so that the penetrating concentration of oil is very low.Oil in the waste water is constantly concentrated in circulation groove, and water-soluble small-molecule substance and water molecules become penetrating fluid through fenestra, and the content of oil is very low in the penetrating fluid, usually less than processed waste water 1%.
The present invention adopts the inorganic ceramic membrane filtration technique to process edible oil wastewater, and processed waste water is applied in the fat degumming, not only reduces the pollution to environment, and economizes on resources and the energy.
Summary of the invention:
The environmental pollution that causes in order to reduce the discharging of alkali refining washing waste water, reduce industrial treatment waste water production cost, the invention provides that a kind of to have technique simple, operational safety, pollute less, a kind of suitable suitability for industrialized production of less investment process the alkali refining washing waste water with inorganic ceramic film, and be applied to soybean oil and come unstuck in the process.
The technical scheme that technical solution problem of the present invention adopts is: a kind of method of coming unstuck for soybean oil with inorganic ceramic film processing alkali refining waste water, and its processing step is as follows:
Step 1: the alkali refining washing waste water is added storage tank, squeezing into the ceramic membrane aperture by recycle pump is that the assembly of 0.01~0.8 μ m carries out cross flow filter, filtration pressure difference is that 0.1~0.7MPa, temperature are 30~80 ℃, and penetrating fluid is gone out by the components side surface current, and trapped fluid flows back in the storage tank;
Step 2: crude oil is warming up to 75 ℃, the heavy concentration of adding oil is 85% food grade phosphoric acid 0.2%, rapid stirring 1~2min, the alkali refining washing waste water of adding behind the inorganic ceramic membrane filtration is that penetrating fluid is that oil is heavy by 14%, the reaction of under the stirring of 60r/min, coming unstuck, reaction times 30min, 78 ℃ of temperature of reaction, centrifugation is got the upper strata degummed oil for subsequent use;
Step 3: accurately take by weighing 300g appeal degummed oil, be heated to 50 ℃, add 45% citric acid 0.36ml, homogeneous 1min, keep 20min under 50 ℃ of water-bath 500r/min mechanical stirring, be cooled to 40 ℃, add 4%NaOH and transfer pH to 5.0, add again the washing waste water behind a certain amount of ceramic membrane filter, with a certain amount of phospholipase A1, water-bath a few hours under certain speed conditions, then centrifugation is got the upper strata degummed oil and is surveyed its phosphorus content;
Step 4: select that the washing waste water behind the ceramic membrane filter weighs 1~4% for oil in the process of coming unstuck, the same step 3 of process, the washing waste water addition behind the process ceramic membrane filter of determining to come unstuck;
Step 5: select the concentration 10~70mg/kg of phospholipase A1 in the process of coming unstuck, the same step 1 of process is determined the enzyme liquid concentration of the process of coming unstuck;
Step 6: stirring velocity is 60~140r/min in the process of selecting to come unstuck, the same step 1 of process, the process stirring velocity of determining to come unstuck;
Step 7: the selection usually time is 1~6h, and the same step 1 of process is determined usually time;
Step 8: the temperature of selecting to come unstuck is 40~70 ℃, and the same step 1 of process is determined the temperature of coming unstuck.
Useful point of the present invention is:
1, adopt the alkali refining washing waste water to come unstuck, under gauge pressure 300kPa condition, soybean processing oil can be saved 0.016 ton of/ton oil of steam consumption.
2, the pH8.8 of alkali refining washing waste water, saponified matter content 0.80%, the washing waste water pH7.5 of oleaginousness 2000mg/L after ceramic membrane is processed, saponified matter content 0.67%, oleaginousness 9.1mg/L has significantly reduced the loss of grease after ceramic membrane is processed.
3, be dissolved with the alkali of fatty acid sodium soap and excess in the washing waste water, as directly entering the river, not only cause water-quality deterioration, affect the existence of organism in water, but also affect agricultural irrigation and the resident drinks, cause environmental pollution.And the present invention is well utilized washing waste water, and the phosphorus content that records after coming unstuck is about 5mg/kg, and is also more desirable than the degumming effect of in the past Degumming method.
Embodiment:
Embodiment one: the step of present embodiment is as follows:
Step 1: the alkali refining washing waste water is added storage tank, squeezing into the ceramic membrane aperture by recycle pump is that the assembly of 0.01~0.8 μ m carries out cross flow filter, filtration pressure difference is that 0.1~0.7MPa, temperature are 30~80 ℃, and penetrating fluid is gone out by the components side surface current, and trapped fluid flows back in the storage tank;
Step 2: crude oil is warming up to 75 ℃, the heavy concentration of adding oil is 85% food grade phosphoric acid 0.2%, rapid stirring 1~2min, the alkali refining washing waste water of adding behind the inorganic ceramic membrane filtration is that penetrating fluid is that oil is heavy by 14%, the reaction of under the stirring of 60r/min, coming unstuck, reaction times 30min, 78 ℃ of temperature of reaction, centrifugation is got the upper strata degummed oil for subsequent use;
Step 3: accurately take by weighing 300g appeal degummed oil, be heated to 50 ℃, add 45% citric acid 0.36ml, homogeneous 1min, keep 20min under 50 ℃ of water-bath 500r/min mechanical stirring, be cooled to 40 ℃, add 4%NaOH and transfer pH to 5.0, add again the washing waste water behind a certain amount of ceramic membrane filter, with a certain amount of phospholipase A1, water-bath a few hours under certain speed conditions, then centrifugation is got the upper strata degummed oil and is surveyed its phosphorus content;
Step 4: select that the washing waste water behind the ceramic membrane filter weighs 1~4% for oil in the process of coming unstuck, the same step 3 of process, the washing waste water addition behind the process ceramic membrane filter of determining to come unstuck;
Step 5: select the addition of phospholipase A1 in the process of coming unstuck to be 10~70mg/kg of oil, the same step 1 of process is determined the enzyme liquid concentration of the process of coming unstuck;
Step 6: stirring velocity is 60~140r/min in the process of selecting to come unstuck, the same step 1 of process, the process stirring velocity of determining to come unstuck;
Step 7: the selection usually time is 1~6h, and the same step 1 of process is determined usually time;
Step 8: the temperature of selecting to come unstuck is 40~70 ℃, and the same step 1 of process is determined the temperature of coming unstuck.
Specific implementation method two: this implementation method is that with specific implementation method one difference step 1 ceramic membrane aperture is 0.01~0.2 μ m, and filtration pressure difference is that 0.1~0.3MPa, temperature are 40~70 ℃, and other composition is identical with specific implementation method one with step.
Specific implementation method three: this implementation method is that with specific implementation method one difference the washing waste water behind the selection ceramic membrane filter weighs 1~3% for oil in the step 4, and other composition is identical with specific implementation method one with step.
Specific implementation method four: this implementation method is to select in the step 5 addition of phospholipase A1 to be 20~50mg/kg of oil with specific implementation method one difference, and other composition is identical with specific implementation method one with step.
Specific implementation method five: this implementation method is to select in the step 6 stirring velocity to be respectively 80~120r/min with specific implementation method one difference, and other composition is identical with specific implementation method one with step.
Specific implementation method six: this implementation method is that with specific implementation method one difference the selective reaction time is respectively 2~5h in the step 7, and other composition is identical with specific implementation method one with step.
Specific implementation method seven: this implementation method is that with specific implementation method one difference the selective reaction temperature is 40~50 ℃ in the step 8, and other composition is identical with specific implementation method one with step.

Claims (7)

1. process alkali refining waste water with inorganic ceramic film and be used for the method that soybean oil is come unstuck for one kind, it is characterized in that its processing step is as follows:
Step 1: the alkali refining washing waste water is added storage tank, squeezing into the ceramic membrane aperture by recycle pump is that the assembly of 0.01~0.8 μ m carries out cross flow filter, filtration pressure difference is that 0.1~0.7MPa, temperature are 30~80 ℃, and penetrating fluid is gone out by the components side surface current, and trapped fluid flows back in the storage tank;
Step 2: crude oil is warming up to 75 ℃, the heavy concentration of adding oil is 85% food grade phosphoric acid 0.2%, rapid stirring 1~2min, the alkali refining washing waste water of adding behind the inorganic ceramic membrane filtration is that penetrating fluid is that oil is heavy by 14%, the reaction of under the stirring of 60r/min, coming unstuck, reaction times 30min, 78 ℃ of temperature of reaction, centrifugation is got the upper strata degummed oil for subsequent use;
Step 3: accurately take by weighing 300g appeal degummed oil, be heated to 50 ℃, add 45% citric acid 0.36ml, homogeneous 1min, keep 20min under 50 ℃ of water-bath 500r/min mechanical stirring, be cooled to 40 ℃, add 4%NaOH and transfer pH to 5.0, add again the washing waste water behind a certain amount of ceramic membrane filter, with a certain amount of phospholipase A1, water-bath a few hours under certain speed conditions, then centrifugation is got the upper strata degummed oil and is surveyed its phosphorus content;
Step 4: select that the washing waste water behind the ceramic membrane filter weighs 1%~4% for oil in the process of coming unstuck, the same step 3 of process, the washing waste water addition behind the process ceramic membrane filter of determining to come unstuck;
Step 5: select the addition of phospholipase A1 in the process of coming unstuck to be 10~70mg/kg of oil, the same step 1 of process is determined the enzyme liquid concentration of the process of coming unstuck;
Step 6: stirring velocity is 60~140r/min in the process of selecting to come unstuck, the same step 1 of process, the process stirring velocity of determining to come unstuck;
Step 7: the selection usually time is 1~6h, and the same step 1 of process is determined usually time;
Step 8: the temperature of selecting to come unstuck is 40~70 ℃, and the same step 1 of process is determined the temperature of coming unstuck.
2. according to claim 1 a kind of with inorganic ceramic film processing alkali refining washing waste water, under certain reaction conditions, carry out the method for soybean oil degumming, it is characterized in that step 1 ceramic membrane aperture is 0.01 μ m, filtration pressure difference is that 0.15MPa, temperature are 60 ℃.
3. according to claim 1 a kind of with inorganic ceramic film processing alkali refining washing waste water, under certain reaction conditions, carry out the method for soybean oil degumming, it is characterized in that the washing waste water behind the selection ceramic membrane filter weighs 2% for oil in the step 4.
4. according to claim 1 a kind of with inorganic ceramic film processing alkali refining washing waste water, under certain reaction conditions, carry out the method for soybean oil degumming, it is characterized in that selecting in the step 5 addition of phospholipase A1 to be the 30mg/kg of oil.
5. according to claim 1 a kind of with inorganic ceramic film processing alkali refining washing waste water, under certain reaction conditions, carry out the method for soybean oil degumming, it is characterized in that selecting stirring velocity in the step 6 is 100r/min.
6. according to claim 1 a kind of with inorganic ceramic film processing alkali refining washing waste water, under certain reaction conditions, carry out the method for soybean oil degumming, it is characterized in that the selective reaction time is 4h in the step 7.
7. according to claim 1 a kind of with inorganic ceramic film processing alkali refining washing waste water, under certain reaction conditions, carry out the method for soybean oil degumming, it is characterized in that the selective reaction temperature is 45 ℃ in the step 8.
CN2012103785476A 2012-09-21 2012-09-21 Soybean oil degumming method utilizing alkali refining waste water treated by inorganic ceramic membrane Pending CN102876452A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105016522A (en) * 2015-07-06 2015-11-04 郑州大学综合设计研究院有限公司 Film treatment process for fatty acid wastewater

Citations (4)

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Publication number Priority date Publication date Assignee Title
JPH11228986A (en) * 1998-02-10 1999-08-24 Agency Of Ind Science & Technol Degumming method with phospholipase
US20080182322A1 (en) * 2007-01-30 2008-07-31 Dayton Christopher L G Enzymatic Degumming Utilizing a Mixture of PLA and PLC Phospholipases
CN101731368A (en) * 2010-02-01 2010-06-16 东北农业大学 Method for substituting washing wastewater of oil alkali refining for hydrated hot water
CN101760298A (en) * 2010-02-01 2010-06-30 东北农业大学 Method of refining fat in alkali by washing wastewater for degumming

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11228986A (en) * 1998-02-10 1999-08-24 Agency Of Ind Science & Technol Degumming method with phospholipase
US20080182322A1 (en) * 2007-01-30 2008-07-31 Dayton Christopher L G Enzymatic Degumming Utilizing a Mixture of PLA and PLC Phospholipases
CN101731368A (en) * 2010-02-01 2010-06-16 东北农业大学 Method for substituting washing wastewater of oil alkali refining for hydrated hot water
CN101760298A (en) * 2010-02-01 2010-06-30 东北农业大学 Method of refining fat in alkali by washing wastewater for degumming

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105016522A (en) * 2015-07-06 2015-11-04 郑州大学综合设计研究院有限公司 Film treatment process for fatty acid wastewater
CN105016522B (en) * 2015-07-06 2017-05-10 郑州大学综合设计研究院有限公司 Film treatment process for fatty acid wastewater

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Application publication date: 20130116