CN106187689B - A kind of method of continuous purification crude glycerine - Google Patents
A kind of method of continuous purification crude glycerine Download PDFInfo
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- CN106187689B CN106187689B CN201610662963.7A CN201610662963A CN106187689B CN 106187689 B CN106187689 B CN 106187689B CN 201610662963 A CN201610662963 A CN 201610662963A CN 106187689 B CN106187689 B CN 106187689B
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- tower
- hydraulic separators
- cyclone hydraulic
- reboiler
- glycerol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of method for serialization purifying crude glycerol, tower bottom of rectifying tower is also connected with cyclone hydraulic separators in addition to connecting reboiler；The feed inlet of cyclone hydraulic separators is connected with tower reactor, and overflow port is connected with reboiler material inlet.Circulating pump is set between tower reactor and cyclone hydraulic separators.By the crude glycerine after taking off gently, it is sent into rectifying column, overhead extraction glycerol product, kettle material is continuously discharged in tower reactor-cyclone hydraulic separators-reboiler cyclic process, from hydrocyclone underflow mouth containing dense salt residue.165~180 DEG C of tower bottom of rectifying tower temperature, 0.001~0.002MPa of pressure.The method of purifying crude glycerol mixture of the invention is carried out continuously, especially suitable for industrialized production.Compared with the prior art, it is carried out in conventional equipment, does not need to invest special equipment, this is compared with art methods with advantage economically.
Description
Technical field
The present invention relates to a kind of methods for serialization purifying crude glycerol, more particularly to as from vegetable oil and tallow
The by-product of fat production biodiesel and the purification treating method of crude glycerine obtained.
Background technique
Glycerol, i.e. Glycerin are present in plant and animal oils and fats with compound state.Especially
Ground, it exists in the form of with the fatty acid such as triglyceride of stearic acid, oleic acid, palmitinic acid and lauric acid chemical combination.
It is most widely used in from plant and animal oils and fats, the commercial run for obtaining glycerol is related to saponification instead
It answers and the ester exchange reaction with alcohols such as ethyl alcohol or methanol.
In general, crude glycerine obtained includes plurality of impurities.It is remaining thick after evaporation recycling excessive methanol or ethyl alcohol
Glycerol generally comprises glycerol, water, inorganic salts (usually sodium salt or sylvite) and non-glycerol organic matter (MONG) and a small amount of alcohol.
The method of refining crude glycerin mainly has ion-exchange, distillation under vacuum and membrane filter method at present.Ion-exchange,
It is first with big described in Chinese patent CN103097327A, Brazilian patent PI8904007 such as United States Patent (USP) US4990695
Amount water or organic solvent dilute crude glycerine, slough in solution after reducing viscosity using multiple anion-cation exchange resin columns
Ion, finally using after rectifying and dewatering, removal of impurities smart glycerol product, this method since a large amount of water or organic solvent is added,
Energy consumption is larger in distillation process.Membrane filter method, such as United States Patent (USP) US5527974, Brazilian patent PI8904007, European patent
Given by EP0358255, patent WO2008/156612, suitable for the removal of impurities of low concentration glycerine water solution, and it is not suitable for gluing
Spend higher crude glycerine.Distillation under vacuum technology maturation, but this needs strict control condition, because being heated approximately at 170~180
DEG C or more the glycerol of high temperature can decompose or polymerize, cause objectionable formation and glycerol recycling yield to reduce.
Based on distillation under vacuum, in order in distillation process, avoid steaming with glycerol, distillation still salinity is excessively high to be led
The kettle temperature of cause increases problem, there is different solutions.
Method described in U.S. patent documents US4655879 (1987) is first to evaporate crude glycerine in rotating thin film
165-180 DEG C and 10-20 millibar whens, distill in device, separation desalination, hereafter the further low stream in falling film evaporator of distillate
Hinder rectifying in column.The rotary film evaporator processing equipment that this method needs, not only expensive expensive but also technical requirements were high.
Document " Xi Yaonian, serialization crude glycerine distillation technique, Chinese oil, the 3rd phase of volume 27 in 2002 ", discloses moral
Triumphant Mu Ruiyasi Kate company of state serialization crude glycerine distillation technique, will take off light crude glycerine first and send distillation column distillation, tower reactor
Saliferous residue send the glycerol in rotary film evaporator recycling residue again, and there is still a need at rotary film evaporator for this method
Equipment is managed, compared with US4655879, since the treating capacity of saliferous object is reduced, the volume of rotary film evaporator is many smaller, but
The depth for distilling column distillation reduces, and rotary film evaporator recycling amounts of glycerol is larger, and energy consumption greatly increases.
Therefore, it is intended that developing one kind, simply commercial run carrys out the purification of glycerol from crude glycerine, and this method is relatively cheap
And it is carried out continuously.Now it has been proved that it is possible that the simple and easy method of clearance carrys out purifying crude glycerol, i.e., in continuous rectification
High concentration saliferous residue is discharged from rectifying tower reactor bottom using cyclone hydraulic separators in Cheng Zhong.Since saliferous residue is continuously to be discharged
, therefore, rectifying and the purifying of entire crude glycerine are carried out continuously.
Summary of the invention
In order to solve problems in the prior art, the present invention is quasi- by using cyclone hydraulic separators, constantly arranges from rectifying tower reactor bottom
High concentration saliferous residue out achievees the purpose that rectifying and the purifying of entire crude glycerine are carried out continuously.
Technical scheme is as follows:
A method of for serialization purifying crude glycerol, tower bottom of rectifying tower is also connected with spinning liquid in addition to connecting reboiler
Separator；The feed inlet of cyclone hydraulic separators is connected with tower reactor, and overflow port is connected with reboiler material inlet.Tower reactor and spinning liquid point
From circulating pump is arranged between device.
By the crude glycerine after taking off gently, it is sent into rectifying column, overhead extraction glycerol product, kettle material is in tower reactor-rotary filter press
In device-reboiler cyclic process, continuously it is discharged from hydrocyclone underflow mouth containing dense salt residue.
165~180 DEG C of tower bottom of rectifying tower temperature, 0.001~0.002MPa of pressure.
The present invention is based on vacuum distillation principle, capital equipment is a rectifying column, and tower reactor is also connected in addition to connecting reboiler
The feed inlet of cyclone hydraulic separators, i.e. cyclone hydraulic separators is connected with tower reactor, and overflow port is connected with reboiler material inlet.Tower reactor with
Forced circulation pump can be added between cyclone hydraulic separators, enhance the mobility of saliferous material.After light (light component: water and a small amount of alcohol) being taken off
Crude glycerine is sent into the rectifying column, and overhead extraction glycerol product, kettle material is in tower reactor-cyclone hydraulic separators-reboiler cyclic process
In, it is continuously discharged from hydrocyclone underflow mouth containing dense salt residue.Realize that the steady and continuous of rectifying column carries out.
The method of purifying crude glycerol mixture of the invention is carried out continuously, especially suitable for industrialized production.It compares
It in the prior art, is carried out in conventional equipment, does not need to invest special equipment, this is compared with art methods has economy
On advantage.
Detailed description of the invention
Fig. 1 is the method schematic diagram of continuous purification crude glycerine.
In attached drawing, parts list represented by the reference numerals are as follows: C1 rectifying column, and E1 rectifying tower reboiler, E2 rectifying column are cold
Condenser, X cyclone hydraulic separators, P circulating pump.
In attached drawing, stream stock representated by each label is as follows: 1 de- light (light component: water and a small amount of alcohol) crude glycerine, 2 rectifying columns
C1 overhead vapours, 3 rectifying column C1 overhead extraction essence glycerol, 4 rectifying column C1 kettle liquids, 5 contain dense salt residue.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and examples.
Main device and the connection type of continuous purification crude glycerine of the invention as shown in Figure 1, device includes rectifying column C1,
Tower reactor is also connected with cyclone hydraulic separators X in addition to connecting reboiler E1.The feed inlet of cyclone hydraulic separators is connected with tower reactor, overflow port
It is connected with reboiler E1 material inlet.It takes off light crude glycerine 1 and is sent into tower bottom of rectifying tower, it is sweet that overhead vapours 2 produces purifying after condensing
Oil product 3, kettle material a part are recycled through cyclone hydraulic separators-reboiler circulation pump P, a part of from hydrocyclone underflow mouth
Continuous discharge contains dense salt residue 5.1.2~1.4g/cm of residue density3。
Embodiment 1
As shown in Figure 1.By handle 10 tons per hour, saliferous 6% it is de- it is light after crude glycerine for, hydrocyclone underflow
The continuous discharge of mouth contains dense salt residue.Set residue density 1.2g/cm3, cyclone hydraulic separators equipment and design parameter are as follows: charging
Flow 800L/min, the diameter 257mm of separator cylindrical portions, overflow diameter 77mm, overflow pipe insertion depth 90mm, charging
Mouth diameter 51mm, cylinder height 51.3cm, underflow outlet diameter 51mm, total height 128mm.
Embodiment 2
As shown in Figure 1.By handle 10 tons per hour, saliferous 6% it is de- it is light after crude glycerine for, hydrocyclone underflow
The continuous discharge of mouth contains dense salt residue.Set residue density 1.4g/cm3, cyclone hydraulic separators equipment and design parameter are as follows: charging
Flow 800L/min, the diameter 220mm of separator cylindrical portions, overflow diameter 65mm, overflow pipe insertion depth 76mm, charging
Mouth diameter 43mm, cylinder height 433mm, underflow outlet diameter 43mm, total height 108mm.
Embodiment 3
As shown in Figure 1.By handle 15 tons per hour, saliferous 6% it is de- it is light after crude glycerine for, hydrocyclone underflow
The continuous discharge of mouth contains dense salt residue.Set residue density 1.2g/cm3, cyclone hydraulic separators equipment and design parameter are as follows: charging
Flow 1000L/min, the diameter 280mm of separator cylindrical portions, overflow diameter 85mm, overflow pipe insertion depth 98mm, into
Material mouth diameter 56mm, cylinder height 560mm, underflow outlet diameter 56mm, total height 140mm.
Embodiment 4
As shown in Figure 1.By handle 15 tons per hour, saliferous 6% it is de- it is light after crude glycerine for, hydrocyclone underflow
The continuous discharge of mouth contains dense salt residue.Set residue density 1.4g/cm3, cyclone hydraulic separators equipment and design parameter are as follows: charging
Flow 1000L/min, the diameter 237mm of separator cylindrical portions, overflow diameter 71mm, overflow pipe insertion depth 83mm, into
Material mouth diameter 47mm, cylinder height 474mm, underflow outlet diameter 47mm, total height 118mm.
For those skilled in the art, it should be appreciated that represent the present inventor to devices above application and invented
Technology, work well in an embodiment of the present invention, and thus it is considered that these technological maheups its implement it is excellent
Lectotype.But it will be understood by those skilled in the art that these disclosures are based on, in the feelings without departing from the scope of the invention
Under condition, many changes, and still available same or like knot can be carried out to specific embodiment disclosed herein
Fruit.
Claims (2)
1. a kind of method for serialization purifying crude glycerol, it is characterized in that tower bottom of rectifying tower is also connected in addition to connecting reboiler
There is cyclone hydraulic separators；The feed inlet of cyclone hydraulic separators is connected with tower reactor, and overflow port is connected with reboiler material inlet；Tower reactor with
Circulating pump is set between cyclone hydraulic separators；By the crude glycerine after taking off gently, it is sent into rectifying column, overhead extraction glycerol product, kettle material
In tower reactor-cyclone hydraulic separators-reboiler cyclic process, continuously it is discharged from hydrocyclone underflow mouth containing dense salt residue.
2. the method for purifying crude glycerol as described in claim 1, it is characterized in that 165~180 DEG C of tower bottom of rectifying tower temperature, pressure
0.001~0.002MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610662963.7A CN106187689B (en) | 2016-08-10 | 2016-08-10 | A kind of method of continuous purification crude glycerine |
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| CN201610662963.7A CN106187689B (en) | 2016-08-10 | 2016-08-10 | A kind of method of continuous purification crude glycerine |
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| CN106187689B true CN106187689B (en) | 2019-02-22 |
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Families Citing this family (2)
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| CN108069828A (en) * | 2018-01-09 | 2018-05-25 | 山东福富新材料科技有限公司 | A kind of production biodiesel byproduct crude glycerin high-purity purification technique |
| CN111957062A (en) * | 2020-09-11 | 2020-11-20 | 赵汇川 | Reduced pressure distillation device and process for continuous desalting of crude glycerol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4655879A (en) * | 1983-10-28 | 1987-04-07 | Henkel Kommanditgesellschaft Auf Aktien | Glycerol distillation process |
| CN103341273A (en) * | 2013-07-04 | 2013-10-09 | 东南大学 | Platy blister catalytic rectifying tower and production method of biodiesel by catalytic distillation |
| CN104844420A (en) * | 2015-01-21 | 2015-08-19 | 青岛科技大学 | Continuous treatment process and device of neopentyl glycol condensed washing mother liquor |
-
2016
- 2016-08-10 CN CN201610662963.7A patent/CN106187689B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4655879A (en) * | 1983-10-28 | 1987-04-07 | Henkel Kommanditgesellschaft Auf Aktien | Glycerol distillation process |
| CN103341273A (en) * | 2013-07-04 | 2013-10-09 | 东南大学 | Platy blister catalytic rectifying tower and production method of biodiesel by catalytic distillation |
| CN104844420A (en) * | 2015-01-21 | 2015-08-19 | 青岛科技大学 | Continuous treatment process and device of neopentyl glycol condensed washing mother liquor |
Non-Patent Citations (3)
| Title |
|---|
| "甘油薄膜蒸馏技术的研究";施念康等;《日用化学工业》;19860630(第8期);第17页 |
| "皂化甘油蒸馏残渣回收及蒸馏工艺改造";蒋拥军;《中国洗涤用品工业》;20110415(第2期);第63页 |
| "连续化粗甘油蒸馏技术";忻耀年;《中国油脂》;20020630;第27卷(第3期);第67-69页 |
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