CN105154225A - Dry fractionation method for swill-cooked dirty oil fatty acid methyl ester - Google Patents

Dry fractionation method for swill-cooked dirty oil fatty acid methyl ester Download PDF

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Publication number
CN105154225A
CN105154225A CN201510644054.6A CN201510644054A CN105154225A CN 105154225 A CN105154225 A CN 105154225A CN 201510644054 A CN201510644054 A CN 201510644054A CN 105154225 A CN105154225 A CN 105154225A
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China
Prior art keywords
methyl ester
fatty acid
acid methyl
controls
oil fatty
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CN201510644054.6A
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Chinese (zh)
Inventor
钟民强
邓金华
汤志刚
李庆
鲁昊
张应赤
王度兵
易超华
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HUBEI TIANJI BIOENERGY TECHNOLOGY DEVELOPMENT Co Ltd
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HUBEI TIANJI BIOENERGY TECHNOLOGY DEVELOPMENT Co Ltd
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Priority to CN201510644054.6A priority Critical patent/CN105154225A/en
Publication of CN105154225A publication Critical patent/CN105154225A/en
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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a dry fractionation method for swill-cooked dirty oil fatty acid methyl ester. The dry fractionation method comprises the following steps: putting a mixed swill-cooked dirty oil fatty acid methyl ester liquid to be fractionated into a storage tank equipped with a stirrer for temperature controlled storage; pumping the stored liquid into a crystallization tank equipped with a stirrer; cooling slowly and carrying out stirring; freezing for crystallization to obtain mixed methyl ester slurry; pumping the mixed methyl ester slurry into a diaphragm filter press with a two-stage single-screw pump for filter pressing; collecting the filtrate; putting the filtrate into an unsaturated fatty acid methyl ester tank for storage; blowing compressed air into a mixed methyl ester slurry inlet to recycle methyl ester slurry for use; heating the saturated fatty acid methyl ester cake obtained through filter pressing for melting; pumping the melted product into the storage tank for storage. The method is a novel way for separating saturated fatty acid methyl ester and unsaturated fatty acid methyl ester of swill-cooked dirty oil fatty acid methyl ester, and has the advantages that the technological operation is easy; the product yield is high; the product quality is stable; the operation cost is low.

Description

A kind of dry fractionation method of sewer oil fatty acid methyl ester
Technical field
The present invention relates to chemical field, specifically a kind of dry fractionation method of sewer oil fatty acid methyl ester.
Background technology
At present, due to the fast development of economy, the standard of living of people also improves fast, and food service industry is also in fast development.In catering industry, people are also producing a large amount of sewer oils while enjoying delicious food indirectly.Be at present all simply be separated for trench oil handling, but along with the quick generation of sewer oil, existing sewer oil treatment process can not meet the needs of modern development.Due to Methyl palmitoleinate and Uniphat A60 in sewer oil fatty acid methyl ester, Witconol 2301 and methyl stearate have identical carbon-chain structure, therefore cannot realize being separated by existing rectifying separation method, therefore sewer oil is caused to reclaim difficulty, not only cause the pollution of sewer oil, and cause the waste of the energy.And there is no Patents or the open separation method about these materials in sewer oil of document.
The zero pour of sewer oil fatty acid methyl ester admixture generally at about 3 DEG C, classical group prejudice table 1,
Table 1 sewer oil fatty acid methyl ester typical case composition
Project Content (%) Fusing point DEG C
Beans bandit acid methyl esters 0.5 18.0
Uniphat A60 19.2 28.0
Methyl palmitoleinate 1.5 -20.0
Methyl stearate 6.8 38.0
Witconol 2301 39.1 -19.9
Methyl linoleate 30.2 -35
Linolenic acid methylester 2.3 -45.5
Other 0.4
The crystallisation by cooling process of mixed methyl aliphatic ester, process of cooling is the crystal habit controlling solid fatty acid methyl esters in mixed methyl aliphatic ester, and the form of crystallization determines the quality of filtration, the process of cooling therefore controlling mixed methyl seems particularly important in dry fractionation technique.
Summary of the invention
The present invention is based on dissimilar fatty acid methyl ester different melting points or its mutual solubility is different at different temperature, a kind of dry fractionation method of sewer oil fatty acid methyl ester is provided, make saturated fatty acid methyl ester crystallisation by cooling, then solid-liquid separation and reach point object put forward, to solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
A dry fractionation method for sewer oil fatty acid methyl ester, concrete steps are as follows:
(1) will treat that point mixing trench soyate liquid carried is put into the hold-up vessel that agitator is housed and carried out temperature control storage, temperature controls at 10 ~ 60 DEG C, and stirring velocity controls at 0 ~ 60 turn/min;
(2) be equipped with in the crystallizer of agitator by raw material toothed gear pump feeding, slow cooling also stirs, and carries out freezing and crystallizing, rate of temperature fall controls at 2 ~ 10 DEG C/h, Tc controls at-5 ~ 5 DEG C, and freezing and crystallizing time controling is at 10 ~ 24h, and stirring velocity controls at 0 ~ 45 turn/min;
(3) adopt twin-stage mono-pump to carry in the mixed methyl slurry completing crystallization, discharge crystallizer, the frequency control of continus convergence is at 0 ~ 60Hz, and the pressure-controlling of twin-stage mono-pump is at 0 ~ 1.8MPa;
(4) be input in barrier film press filtration squeezing machine and carry out press filtration by mixed methyl slurry, the pressure-controlling of press filtration is at 0 ~ 1.5MPa, and the pressure-controlling of diaphragm pressing is at 1 ~ 4.0MPa;
(5) store in the filtrate collection be press-filtered out feeding unsaturated fatty acid methyl ester tank;
(6) be blown into pressurized air to reclaim methyl acrylate paste to the mixed methyl slurry entrance after press filtration, and deliver in raw material storage tanks and recycle;
(7) saturated fatty acid methyl ester cake heat fused press filtration obtained, is pumped in hold-up vessel and stores.
As the further scheme of the present invention: in step (1), temperature controls at 20 ~ 40 DEG C, and stirring velocity controls at 15 ~ 25 turns/min.
As the further scheme of the present invention: in step (2), rate of temperature fall controls at 4 ~ 6 DEG C/h, and Tc controls at-1 ~ 1 DEG C, and freezing and crystallizing time controling is at 15 ~ 18h, and stirring velocity controls at 12 ~ 18 turns/min.
As the further scheme of the present invention: in step (3), the frequency control of continus convergence is at 30 ~ 40Hz, and the pressure-controlling of twin-stage mono-pump is at 1.0 ~ 1.2MPa.
As the present invention's further scheme: in step (4), the pressure-controlling of press filtration is at 0.6 ~ 1.0MPa, and the pressure-controlling of diaphragm pressing is at 2.8 ~ 3.0MPa.
Compared with prior art, the invention has the beneficial effects as follows: the new way that the inventive method sewer oil fatty acid methyl ester saturated fatty acid methyl ester is separated with unsaturated fatty acid methyl ester, have technological operation easy, product yield is high, constant product quality, the advantage that process cost is low.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The dry fractionation method of sewer oil fatty acid methyl ester, concrete steps are as follows:
(1) will treat that point mixing trench soyate liquid carried is put into the hold-up vessel that agitator is housed and carried out temperature control storage, temperature controls at 30 ~ 35 DEG C, and stirring velocity is 25 turns/min;
(2) be equipped with in the crystallizer of agitator by raw material toothed gear pump feeding, slow cooling also stirs, and carry out freezing and crystallizing, crystallizer has 8m 2/ m 3cooling area, stirring velocity program follows principle first quick and back slow, adopts different stirring velocitys in differing temps section, with guarantee product maximum homogeneity and in whole crystallisation process efficient thermal energy exchange, crystallizer chuck is with water circulation system; In crystallisation by cooling process, the temperature of mixed methyl slurry and water is all passed through and is measured and record; The temperature of water coolant controls, and adopts correspondence progressively program process control, guarantees to carry out crystallization on predetermined cooling curve;
Rate of temperature fall controls at 4 ~ 6 DEG C/h, and Tc controls at-1 ~ 1 DEG C, and freezing and crystallizing time controling is at 15 ~ 18h, and stirring velocity controls, at 12 ~ 18 turns/min, to obtain uniform xln, easily filters and constitutionally stable methyl acrylate paste;
(3) the mixed methyl slurry crystal grain that crystallisation by cooling is formed is only the xln under methyl esters different melting points, and its structural strength is limited, can not bear high-shear and pressure, avoids as far as possible producing turbulent shear and destroying crystal in course of conveying; Adopt little (1.2MPa) twin-stage mono-pump of shearing force to carry in the mixed methyl slurry completing crystallization, the mixed methyl slurry completing crystallization is discharged from crystallizer by spiral pump,
Wherein, the frequency control of continus convergence is at 0 ~ 60Hz, and the pressure-controlling of twin-stage mono-pump is at 0 ~ 1.8MPa; The frequency control of continus convergence is at 30 ~ 40Hz, and the pressure-controlling of twin-stage mono-pump is at 1.0 ~ 1.2MPa.
(4) be input in barrier film press filtration squeezing machine and carry out press filtration by mixed methyl slurry, barrier film press filtration squeezing machine is that the space bar used by screen plate, barrier film and exchange assembles up; Mixed methyl slurry will enter all intervals, and by each block screen plate, liquid unsaturated fatty acid methyl ester is flowed out by filter cloth, remaining solid acid, shift space bar with the pressurization of liquid gas onto from diaphragm plate back to squeeze, filtrate collection sends into unsaturated fatty acid methyl ester basin
Wherein, the pressure-controlling of press filtration is at 0.8 ~ 1.0MPa, and the pressure-controlling of diaphragm pressing is at 2.8 ~ 3.0MPa;
(5) store in the filtrate collection be press-filtered out feeding unsaturated fatty acid methyl ester tank;
(6) be blown into pressurized air to reclaim methyl acrylate paste to the mixed methyl slurry entrance after press filtration, and deliver in raw material storage tanks and recycle;
(7) saturated fatty acid methyl ester cake heat fused press filtration obtained, is pumped in hold-up vessel and stores, and filter cloth needs regularly with hot unsaturated fatty acid methyl ester cleaning and the solid melts be bonded on cloth.
Table 2 unsaturated fatty acid methyl ester component
Project Content (%) Content (%) Content (%)
Uniphat A60 1.3 1.1 1.2
Methyl palmitoleinate 1.8 1.7 2.0
Methyl stearate 0.6 0.5 0.7
Witconol 2301 52.0 53.3 51.8
Methyl linoleate 41.3 40.6 41.0
Methyl linoleate 3.0 2.8 3.3
Add up to 100 100 100
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.

Claims (5)

1. a dry fractionation method for sewer oil fatty acid methyl ester, it is characterized in that, concrete steps are as follows:
(1) will treat that point mixing trench soyate liquid carried is put into the hold-up vessel that agitator is housed and carried out temperature control storage, temperature controls at 10 ~ 60 DEG C, and stirring velocity controls at 0 ~ 60 turn/min;
(2) be equipped with in the crystallizer of agitator by raw material toothed gear pump feeding, slow cooling also stirs, and carries out freezing and crystallizing, rate of temperature fall controls at 2 ~ 10 DEG C/h, Tc controls at-5 ~ 5 DEG C, and freezing and crystallizing time controling is at 10 ~ 24h, and stirring velocity controls at 0 ~ 45 turn/min;
(3) adopt twin-stage mono-pump to carry in the mixed methyl slurry completing crystallization, discharge crystallizer, the frequency control of continus convergence is at 0 ~ 60Hz, and the pressure-controlling of twin-stage mono-pump is at 0 ~ 1.8MPa;
(4) be input in barrier film press filtration squeezing machine and carry out press filtration by mixed methyl slurry, the pressure-controlling of press filtration is at 0 ~ 1.5MPa, and the pressure-controlling of diaphragm pressing is at 1 ~ 4.0MPa;
(5) store in the filtrate collection be press-filtered out feeding unsaturated fatty acid methyl ester tank;
(6) be blown into pressurized air to reclaim methyl acrylate paste to the mixed methyl slurry entrance after press filtration, and deliver in raw material storage tanks and recycle;
(7) saturated fatty acid methyl ester cake heat fused press filtration obtained, is pumped in hold-up vessel and stores.
2. the dry fractionation method of sewer oil fatty acid methyl ester according to claim 1, is characterized in that, in step (1), temperature controls at 20 ~ 40 DEG C, and stirring velocity controls at 15 ~ 25 turns/min.
3. the dry fractionation method of sewer oil fatty acid methyl ester according to claim 1, is characterized in that, in step (2), rate of temperature fall controls at 4 ~ 6 DEG C/h, Tc controls at-1 ~ 1 DEG C, and freezing and crystallizing time controling is at 15 ~ 18h, and stirring velocity controls at 12 ~ 18 turns/min.
4. the dry fractionation method of sewer oil fatty acid methyl ester according to claim 1, is characterized in that, in step (3), the frequency control of continus convergence is at 30 ~ 40Hz, and the pressure-controlling of twin-stage mono-pump is at 1.0 ~ 1.2MPa.
5. the dry fractionation method of sewer oil fatty acid methyl ester according to claim 1, is characterized in that, in step (4), the pressure-controlling of press filtration is at 0.6 ~ 1.0MPa, and the pressure-controlling of diaphragm pressing is at 2.8 ~ 3.0MPa.
CN201510644054.6A 2015-10-09 2015-10-09 Dry fractionation method for swill-cooked dirty oil fatty acid methyl ester Pending CN105154225A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107840800A (en) * 2016-09-19 2018-03-27 北京林氏精化新材料有限公司 A kind of cryogenic purincation separating technology of the fatty acid ester of low-carbon alcohol class plasticizer based on palm oil
CN109971551A (en) * 2019-03-28 2019-07-05 福建省明洲环保发展有限公司 A kind of method and product preparing environmentally friendly chloro plasticizer by waste grease
CN109971552A (en) * 2019-03-28 2019-07-05 浙江嘉澳环保科技股份有限公司 A method of epoxy plasticizer and chloro plasticizer are prepared by waste grease

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107840800A (en) * 2016-09-19 2018-03-27 北京林氏精化新材料有限公司 A kind of cryogenic purincation separating technology of the fatty acid ester of low-carbon alcohol class plasticizer based on palm oil
CN109971551A (en) * 2019-03-28 2019-07-05 福建省明洲环保发展有限公司 A kind of method and product preparing environmentally friendly chloro plasticizer by waste grease
CN109971552A (en) * 2019-03-28 2019-07-05 浙江嘉澳环保科技股份有限公司 A method of epoxy plasticizer and chloro plasticizer are prepared by waste grease
CN109971551B (en) * 2019-03-28 2022-09-20 福建省明洲环保发展有限公司 Method for preparing environment-friendly chlorinated plasticizer from waste oil and fat and product
CN109971552B (en) * 2019-03-28 2022-12-02 浙江嘉澳环保科技股份有限公司 Method for preparing epoxy plasticizer and chlorinated plasticizer from waste grease

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