CN103172851A - Method for preparing polyglycerol fatty acid ester with illegal cooking oil - Google Patents
Method for preparing polyglycerol fatty acid ester with illegal cooking oil Download PDFInfo
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- CN103172851A CN103172851A CN2013100927501A CN201310092750A CN103172851A CN 103172851 A CN103172851 A CN 103172851A CN 2013100927501 A CN2013100927501 A CN 2013100927501A CN 201310092750 A CN201310092750 A CN 201310092750A CN 103172851 A CN103172851 A CN 103172851A
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Abstract
The invention belongs to the preparation method for polyglycerol ester, and in particular relates to a method for preparing polyglycerol fatty acid ester with illegal cooking oil. The method comprises the following steps of firstly pretreating the illegal cooking oil; sending the pretreated illegal cooking oil and water into a hydrolysis reaction kettle to enable the illegal cooking oil to have hydrolysis reaction at high temperature and under acidic condition, so as to obtain fatty acid, water vapor, crude glycerin and oil; after the fatty acid and the water vapor flow back through condensation, redistilling so as to remove the water vapor to obtain a fatty acid product; and finally obtaining the refined glycerin after separation, centrifugal purification and refining of the crude glycerin, obtaining polyglycerol after polymerization reaction of the refined glycerin, and finally sending the polyglycerol and fatty acid into an esterification reaction kettle for esterification reaction at high temperature and under the alkaline condition so as to obtain the polyglycerol fatty acid ester product. According to the preparation method, not only the waste can be turned into wealth, but also waste cooking oil can find a way out so as to be prevented from flowing into oil markets to harm health of people and prevented from flowing into a sewer directly to contaminate the environment.
Description
Technical field
The invention belongs to the preparation method of polyglycerol ester, be specifically related to a kind of method that sewer oil prepares polyglycerol fatty acid ester.
Background technology
Polyglycerol fatty acid ester is called for short polyglycerol ester, is that a class is novel, efficient, the multi-hydroxy ester class nonionic surface active agent of excellent property.Polyglycerol fatty acid ester not only has stronger emulsification, dispersion, permeates and dissolve power, and have the heat-resisting and acid-fast ability stronger than other poly-hydroxy class fatty acid ester, united state food and agricultural organization and the World Health Organization confirm as nontoxic high security foodstuff additive.
Along with developing rapidly of economy, the quantity discharged of China's sewer oil also increases rapidly thereupon.Because China comparatively effectively recycles approach to the trench oil starvation at present, some lawless persons to refine the sewer oil that reclaims, and make it to return dining table by back door, and then serve as people's daily edible oil in order to seek exorbitant profit.Yet owing to containing a large amount of poisonous carcinogenic compositions in sewer oil, long-term eating can cause food poisoning, even will cause the eater to suffer from cancered serious consequence, thereby serious threat is to people's physical and mental health.Therefore how sewer oil being recycled effectively, is a technical barrier of instantly being badly in need of solving.
Summary of the invention
The object of the present invention is to provide a kind of sewer oil to prepare the method for polyglycerol fatty acid ester, present method utilizes sewer oil to produce polyglycerol fatty acid ester, not only can turn waste into wealth, and avoided sewer oil flow into edible oil market and be detrimental to health, also avoided sewer oil to flow directly into water drain and pollution of ecological environment simultaneously.
For achieving the above object, the present invention has adopted following technical scheme: a kind of sewer oil prepares the method for polyglycerol fatty acid ester, it is characterized in that comprising the following steps:
(1), the sewer oil of 100 weight parts is sent in pretreater, add the hydrogen peroxide of 3～4 weight parts in the pretreater, the temperature of controlling in pretreater is 60 ℃, continuously stirring 20min; Add the atlapulgite of 4～5 weight parts again in pretreater, and pretreater is warming up to 70 ℃, then continuously stirring 20min obtains pretreated sewer oil;
(2), the pretreated sewer oil of preparation in step (1) is sent in hydrolytic reaction pot, add the water of 70～80 weight parts and 1～2 weight part concentration in the hydrolytic reaction pot and be 98% the vitriol oil, the temperature of controlled hydrolysis reactor is 200～250 ℃, pressure is normal pressure, make sewer oil under high temperature, condition of normal pressure with water vapor generation hydrolysis reaction, hydrolysis obtains lipid acid, water vapor, raw glycerine and grease;
(3), the prepared lipid acid of (2) step is entered in condenser with water vapor, after conventional condensation process, then send in distiller, the temperature of controlling distiller is that 100～105 ℃, pressure are normal pressure, separates to get fatty acid product and water; And the raw glycerine in (2) step hydrolytic reaction pot and grease are carried out standing demix, the temperature of controlled hydrolysis reactor is that 60～80 ℃, pressure are normal pressure, collects lower floor's liquid and is the raw glycerine product;
(4), (3) step gained raw glycerine product is sent in whizzer, add the methyl alcohol of 15～20 weight parts to dilute in described raw glycerine product, then centrifugation 15 minutes on whizzer is collected lower floor's liquid and is glycerol semi-final product;
(5), (4) step gained glycerol semi-final product is moved in rectifier, the temperature of controlling rectifier is 70 ℃, and methyl alcohol is reclaimed in air distillation, and 164～204 ℃ of cuts are collected in underpressure distillation, are refining glycerine;
(6), the gained refining glycerine is added in polymerization reaction kettle, pass into nitrogen in polymerization reaction kettle, the temperature of controlling in polymerization reaction kettle is 120 ℃～150 ℃, preheating 10～30 minutes, then the sodium hydroxide or the potassium hydroxide that add 1～2 weight part, and constantly stir, the temperature in polymerization reaction kettle is risen to 220 ℃～250 ℃, reacted 5～6 hours, and obtained the Polyglycerine product;
(7), (6) step gained Polyglycerine product is sent in reaction kettle of the esterification, the sodium hydroxide or the potassium hydroxide that add 1～2 weight part, reaction kettle of the esterification is warming up to 240 ℃, then join (3) step gained fatty acid product in reaction kettle of the esterification in batches, and constantly stir, described fatty acid product added complete in 1.5 hours; Pass into the water vapor of nitrogen remove to generate to reaction kettle of the esterification in above-mentioned reaction process, and constantly analyze acid number, finish reaction when acid number less than 10 the time, cooling rear collection finally obtains the polyglycerol fatty acid ester product.
Simultaneously, the present invention can also be able to further realization by following technical measures:
Preferably, return in the hydrolytic reaction pot of (2) step separating by distiller the water that makes in (3) step, to realize the water circuit utilization.
Preferably, the methyl alcohol that (5) step is reclaimed returns in the whizzer of (4) step, to realize the recycle of methyl alcohol.
Preferably, described sewer oil consist of the natural animal-plant grease, can be used for producing higher fatty acid and glycerine.
Beneficial effect of the present invention is: it is few that present method prepares the by product that polyglycerol fatty acid ester produces, and can realize recycling of material, such as returning in hydrolytic reaction pot after the water process condensation that adds in hydrolysis reaction, distillation, realized the water circuit utilization; The methyl alcohol that is used for the dilution raw glycerine returns to whizzer through after Distillation recovery, has realized recycling of methyl alcohol.Therefore; technical scheme in the present invention is neither outwards discharged any pollutent; can save cost again; improve raw material availability, whole technological process is simple, reaction conditions gentleness and easily control; reaction conversion ratio is high; production process is substantially pollution-free, not only is conducive to environment protection, and comparatively remarkable for the meaning of resource recycling.
Description of drawings
Fig. 1 is structural representation of the present invention.
In figure, the implication of mark is as follows:
1-pretreater, 2-hydrolytic reaction pot, 3-condenser, 4-distiller
5-whizzer, 6-rectifier, 7-polymerization reaction kettle, 8-reaction kettle of the esterification
Embodiment
The present invention will be further described below in conjunction with Figure of description and embodiment.
Embodiment 1
(1), the sewer oil of 100 weight parts is sent in pretreater 1, at first, the hydrogen peroxide that adds 4 weight parts in the described sewer oil, the temperature of controlling pretreater 1 is 60 ℃, continuously stirring 20min, the atlapulgite that adds again matter 5 weight parts is warming up to 70 ℃ with pretreater, then continuously stirring 20min obtains the sewer oil that pre-treatment is received;
(2), the pretreated sewer oil of step (1) preparation is sent in hydrolytic reaction pot 2, add wherein the water of 80 weight parts and 2 weight part concentration and be 98% the vitriol oil, the described vitriol oil is catalyzer, the temperature of controlled hydrolysis reactor 2 is 200～250 ℃, pressure is normal pressure, make sewer oil under high temperature, condition of normal pressure with water vapor generation hydrolysis reaction, hydrolysis obtains lipid acid, water vapor, raw glycerine and grease;
(3), (2) step gained lipid acid is entered in condenser 3 with water vapor, after conventional condensation, then enter in distiller 4, the temperature of controlling distiller 4 is that 100～105 ℃, pressure are normal pressure, separates to get fatty acid product and water;
(4), (3) step separated the water obtain return in the hydrolytic reaction pot 2 of (2) step, realize the water circuit utilization;
(5), the raw glycerine in (2) step hydrolytic reaction pot 2 and grease are carried out standing demix, the temperature of controlled hydrolysis reactor 2 is that 60～80 ℃, pressure are normal pressure, collects lower floor's liquid and is the raw glycerine product;
(6), (5) step gained raw glycerine product is sent in whizzer 5, add the methyl alcohol of 20 weight parts to dilute in described raw glycerine product, centrifugation is 15 minutes on whizzer 5, collects lower floor's liquid and is glycerol semi-final product;
(7), (6) step gained glycerol semi-final product is moved in rectifier 6, the temperature of controlling rectifier 6 is 70 ℃, and methyl alcohol is reclaimed in air distillation, and 164～204 ℃ of cuts are collected in underpressure distillation, are refining glycerine;
(8), methyl alcohol that (7) step is reclaimed returns in the whizzer 5 of (6) step, realizes the recycle of methyl alcohol;
(9), (7) step gained refining glycerine is added in polymerization reaction kettle 7, at first, pass into nitrogen, the temperature of controlling polymerization reaction kettle 7 is 120 ℃～150 ℃, preheating 10～30 minutes, then the sodium hydroxide that adds 2 weight parts, described sodium hydroxide is catalyzer, and constantly stirs, and the temperature of polymerization reaction kettle 7 is risen to 220 ℃～250 ℃, reacted 5～6 hours, and obtained the Polyglycerine product;
(10), (9) step gained Polyglycerine product is sent in reaction kettle of the esterification 8, the sodium hydroxide that adds 2 weight parts, described sodium hydroxide is catalyzer, reaction kettle of the esterification 8 is warming up to 240 ℃ of left and right, (3) step gained fatty acid product is joined in reaction kettle of the esterification 8 in batches, and constantly stir, described fatty acid product added in 1.5 hours; Pass into to reaction kettle of the esterification 8 water vapor that nitrogen remove to generate in reaction process, and constantly analyze acid number, finish reaction, the final polyglycerol fatty acid ester product of cooling rear collection when acid number less than 10 the time.
(1), the sewer oil of 100 weight parts is sent in pretreater 1, at first, the hydrogen peroxide that adds 3 weight parts in the sewer oil, controlling the pretreater temperature is 60 ℃, continuously stirring 20min, the atlapulgite that adds again 4 weight parts is warming up to 70 ℃ with pretreater, then continuously stirring 20min obtains pretreated sewer oil;
(2), the pretreated sewer oil for preparing in step (1) is sent in hydrolytic reaction pot 2, add wherein the water of 80 weight parts and 1 weight part concentration and be 98% the vitriol oil, the described vitriol oil is catalyzer, the temperature of controlled hydrolysis reactor 2 is 200～250 ℃, pressure is normal pressure, make sewer oil under high temperature, condition of normal pressure with water vapor generation hydrolysis reaction, hydrolysis obtains lipid acid, water vapor, raw glycerine and grease;
(3), (2) step gained lipid acid is entered in condenser 3 with water vapor, after conventional condensation, then enter in distiller 4, the temperature of controlling distiller 4 is that 100～105 ℃, pressure are normal pressure, separates to get fatty acid product and water;
(4), water that (3) step is separated returns in the hydrolytic reaction pot 2 of (2) step, realizes the water circuit utilization;
(5), the raw glycerine in the hydrolytic reaction pot 2 of (2) step and grease are carried out standing demix, the temperature of controlled hydrolysis reactor 2 is that 60～80 ℃, pressure are normal pressure, collects lower floor's liquid and is the raw glycerine product;
(6), (5) step gained raw glycerine product is sent in whizzer 5, add the methyl alcohol of 15 weight parts to dilute in described raw glycerine product, centrifugation is 15 minutes on whizzer 5, collects lower floor's liquid and is glycerol semi-final product;
(7), (6) step gained glycerol semi-final product is moved in rectifier 6, the temperature of controlling rectifier 6 is 70 ℃, and methyl alcohol is reclaimed in air distillation, and 164～204 ℃ of cuts are collected in underpressure distillation, are refining glycerine;
(8), methyl alcohol that (7) step is reclaimed returns in the whizzer 5 of (6) step, realizes the recycle of methyl alcohol;
(9), refining glycerine is added in polymerization reaction kettle 7, at first, pass into nitrogen, the temperature of controlling polymerization reaction kettle 7 is 120 ℃～150 ℃, preheating 10～30 minutes, then the sodium hydroxide that adds 1 weight part, described sodium hydroxide is catalyzer, and constantly stirs, and the temperature of polymerization reaction kettle 7 is risen to 220 ℃～250 ℃, reacted 5～6 hours, and obtained the Polyglycerine product;
(10), (9) step gained Polyglycerine product is sent in reaction kettle of the esterification 8, the sodium hydroxide that adds 1 weight part, described sodium hydroxide is catalyzer, reaction kettle of the esterification 8 is warming up to 240 ℃ of left and right, (3) step gained fatty acid product is joined in reaction kettle of the esterification 8 in batches, and constantly stir, described fatty acid product added in 1.5 hours; Pass into to reaction kettle of the esterification 8 water vapor that nitrogen remove to generate in reaction process, and constantly analyze acid number, finish reaction, the final polyglycerol fatty acid ester product of cooling rear collection when acid number less than 10 the time.
(1), the sewer oil of 100 weight parts is sent in pretreater 1, at first, the hydrogen peroxide that adds 3.5 weight parts in the described sewer oil, the temperature of controlling pretreater 1 is 60 ℃, continuously stirring 20min, the atlapulgite that adds again 4.5 weight parts is warming up to 70 ℃ with pretreater 1, then continuously stirring 20min obtains through pretreated sewer oil;
(2), the pretreated sewer oil that step (1) is made is sent in hydrolytic reaction pot 2, add wherein the water of 80 weight parts and 1 weight part concentration and be 98% the vitriol oil, the described vitriol oil is catalyzer, the temperature of controlled hydrolysis reactor 2 is 200～250 ℃, pressure is normal pressure, make sewer oil under high temperature, condition of normal pressure with water vapor generation hydrolysis reaction, hydrolysis obtains lipid acid, water vapor, raw glycerine and grease;
(3), (2) step gained lipid acid is entered in condenser 3 with water vapor, after conventional condensation, then enter in distiller 4, the temperature of controlling distiller 4 is that 100～105 ℃, pressure are normal pressure, separates to get fatty acid product and water;
(4), water that (3) step is separated returns in the hydrolytic reaction pot 2 of (2) step, realizes the water circuit utilization;
(5) raw glycerine in (2) step hydrolytic reaction pot 2 and grease are carried out standing demix, the temperature of controlled hydrolysis reactor 2 is that 60～80 ℃, pressure are normal pressure, collects lower floor's liquid and is the raw glycerine product;
(6), (5) step gained raw glycerine product is sent in whizzer 5, add the methyl alcohol of 17.5 weight parts to dilute in described raw glycerine product, centrifugation is 15 minutes on whizzer 5, collects lower floor's liquid and is glycerol semi-final product;
(7), (6) step gained glycerol semi-final product is moved in rectifier 6, the temperature of controlling rectifier 6 is 70 ℃, and methyl alcohol is reclaimed in air distillation, and 164～204 ℃ of cuts are collected in underpressure distillation, are refining glycerine;
(8), methyl alcohol that (7) step is reclaimed returns in the whizzer 5 of (6) step, realizes the recycle of methyl alcohol;
(9), the refining glycerine that step (7) is made adds in polymerization reaction kettle 7, at first, pass into nitrogen, the temperature of controlling polymerization reaction kettle 7 is 120 ℃～150 ℃, preheating 10～30 minutes, then the potassium hydroxide that adds 1 weight part, described potassium hydroxide is catalyzer, and constantly stirs, and the temperature of polymerization reaction kettle 7 is risen to 220 ℃～250 ℃, reacted 5～6 hours, and obtained the Polyglycerine product;
(10), (9) step gained Polyglycerine product is sent in reaction kettle of the esterification 8, the potassium hydroxide that adds 1 weight part, described potassium hydroxide is catalyzer, reaction kettle of the esterification 8 is warming up to 240 ℃ of left and right, (3) step gained fatty acid product is joined in reaction kettle of the esterification 8 in batches, and constantly stir, described fatty acid product added in 1.5 hours; Pass into to reaction kettle of the esterification 8 water vapor that nitrogen remove to generate in reaction process, and constantly analyze acid number, finish reaction, the final polyglycerol fatty acid ester product of cooling rear collection when acid number less than 10 the time.
Claims (4)
1. a sewer oil prepares the method for polyglycerol fatty acid ester, it is characterized in that comprising the following steps:
(1), the sewer oil of 100 weight parts is sent in pretreater, add the hydrogen peroxide of 3～4 weight parts in the pretreater, the temperature of controlling in pretreater is 60 ℃, continuously stirring 20min; Add the atlapulgite of 4～5 weight parts again in pretreater, and pretreater is warming up to 70 ℃, then continuously stirring 20min obtains pretreated sewer oil;
(2), the pretreated sewer oil of preparation in step (1) is sent in hydrolytic reaction pot, add the water of 70～80 weight parts and 1～2 weight part concentration in the hydrolytic reaction pot and be 98% the vitriol oil, the temperature of controlled hydrolysis reactor is 200～250 ℃, pressure is normal pressure, make sewer oil under high temperature, condition of normal pressure with water vapor generation hydrolysis reaction, hydrolysis obtains lipid acid, water vapor, raw glycerine and grease;
(3), the prepared lipid acid of (2) step is entered in condenser with water vapor, after conventional condensation process, then send in distiller, the temperature of controlling distiller is that 100～105 ℃, pressure are normal pressure, separates to get fatty acid product and water; And the raw glycerine in (2) step hydrolytic reaction pot and grease are carried out standing demix, the temperature of controlled hydrolysis reactor is that 60～80 ℃, pressure are normal pressure, collects lower floor's liquid and is the raw glycerine product;
(4), (3) step gained raw glycerine product is sent in whizzer, add the methyl alcohol of 15～20 weight parts to dilute in described raw glycerine product, then centrifugation 15 minutes on whizzer is collected lower floor's liquid and is glycerol semi-final product;
(5), (4) step gained glycerol semi-final product is moved in rectifier, the temperature of controlling rectifier is 70 ℃, and methyl alcohol is reclaimed in air distillation, and 164～204 ℃ of cuts are collected in underpressure distillation, are refining glycerine;
(6), the gained refining glycerine is added in polymerization reaction kettle, pass into nitrogen in polymerization reaction kettle, the temperature of controlling in polymerization reaction kettle is 120 ℃～150 ℃, preheating 10～30 minutes, then the sodium hydroxide or the potassium hydroxide that add 1～2 weight part, and constantly stir, then the temperature in polymerization reaction kettle is risen to 220 ℃～250 ℃, reacted 5～6 hours, and obtained the Polyglycerine product;
(7), (6) step gained Polyglycerine product is sent in reaction kettle of the esterification, the sodium hydroxide or the potassium hydroxide that add 1～2 weight part, reaction kettle of the esterification is warming up to 240 ℃, then join (3) step gained fatty acid product in reaction kettle of the esterification in batches, and constantly stir, described fatty acid product added complete in 1.5 hours; Pass into the water vapor of nitrogen remove to generate to reaction kettle of the esterification in above-mentioned reaction process, and constantly analyze acid number, finish reaction when acid number less than 10 the time, cooling rear collection finally obtains the polyglycerol fatty acid ester product.
2. sewer oil according to claim 1 prepares the method for polyglycerol fatty acid ester, it is characterized in that: return in the hydrolytic reaction pot of (2) step separating by distiller the water that makes in (3) step, to realize the water circuit utilization.
3. sewer oil according to claim 1 prepares the method for polyglycerol fatty acid ester, it is characterized in that: the methyl alcohol that (5) step is reclaimed returns in the whizzer of (4) step, to realize the recycle of methyl alcohol.
4. sewer oil according to claim 1 prepares the method for polyglycerol fatty acid ester, it is characterized in that: described sewer oil consist of the natural animal-plant grease, can be used for producing higher fatty acid and glycerine.
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Cited By (8)
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| CN103467734A (en) * | 2013-08-12 | 2013-12-25 | 如皋市双马化工有限公司 | Method for preparing polyglyceryl fatty acid ester through using waste oil |
| CN103709415A (en) * | 2013-12-24 | 2014-04-09 | 武汉理工大学 | Preparation method of composite slow-breaking slow-curing asphalt emulsifier |
| CN105670800A (en) * | 2016-04-05 | 2016-06-15 | 浙江宇翔生物科技有限公司 | Method for preparing fatty acid by utilizing illegal cooking oil |
| CN106497680A (en) * | 2016-11-11 | 2017-03-15 | 云南磷化集团有限公司 | A kind of method that oxidation-adsorption purifies food and drink waste oil |
| CN106520381A (en) * | 2016-11-11 | 2017-03-22 | 云南磷化集团有限公司 | Decoloration and deodorization method for drainage oil fatty acid |
| CN107245377A (en) * | 2017-07-31 | 2017-10-13 | 安庆华威油脂科技有限公司 | A kind of trench oil recovery method |
| CN107418726A (en) * | 2017-07-31 | 2017-12-01 | 安庆华威油脂科技有限公司 | A kind of process for purification for reclaiming gutter oil |
| CN108114967A (en) * | 2017-12-20 | 2018-06-05 | 吴豪 | A kind of method that environmental protective soap and sustained release fertilizer are produced using kitchen garbage |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467734A (en) * | 2013-08-12 | 2013-12-25 | 如皋市双马化工有限公司 | Method for preparing polyglyceryl fatty acid ester through using waste oil |
| CN103709415A (en) * | 2013-12-24 | 2014-04-09 | 武汉理工大学 | Preparation method of composite slow-breaking slow-curing asphalt emulsifier |
| CN103709415B (en) * | 2013-12-24 | 2015-07-22 | 武汉理工大学 | Preparation method of composite slow-breaking slow-curing asphalt emulsifier |
| CN105670800A (en) * | 2016-04-05 | 2016-06-15 | 浙江宇翔生物科技有限公司 | Method for preparing fatty acid by utilizing illegal cooking oil |
| CN106497680A (en) * | 2016-11-11 | 2017-03-15 | 云南磷化集团有限公司 | A kind of method that oxidation-adsorption purifies food and drink waste oil |
| CN106520381A (en) * | 2016-11-11 | 2017-03-22 | 云南磷化集团有限公司 | Decoloration and deodorization method for drainage oil fatty acid |
| CN107245377A (en) * | 2017-07-31 | 2017-10-13 | 安庆华威油脂科技有限公司 | A kind of trench oil recovery method |
| CN107418726A (en) * | 2017-07-31 | 2017-12-01 | 安庆华威油脂科技有限公司 | A kind of process for purification for reclaiming gutter oil |
| CN108114967A (en) * | 2017-12-20 | 2018-06-05 | 吴豪 | A kind of method that environmental protective soap and sustained release fertilizer are produced using kitchen garbage |
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Application publication date: 20130626 |