CN104496751B - A kind of processing means for reclaiming glycerol in biodiesel and processing method thereof - Google Patents
A kind of processing means for reclaiming glycerol in biodiesel and processing method thereof Download PDFInfo
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- CN104496751B CN104496751B CN201410754698.6A CN201410754698A CN104496751B CN 104496751 B CN104496751 B CN 104496751B CN 201410754698 A CN201410754698 A CN 201410754698A CN 104496751 B CN104496751 B CN 104496751B
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- 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
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Abstract
nullA kind of processing means for reclaiming glycerol in biodiesel and processing method thereof，By reactor、Methanol recovery device and glycerin treatment tank composition，Described reactor is provided with agitator，The methanol gas outlet arranged at the top of reactor is tightly connected with methanol recovery device，The outer wall of reactor is provided with the heating mantle for being passed through steam，It is arranged on the discharging opening bottom reactor to be connected with glycerin treatment tank by pipeline，Described glycerin treatment tank is provided with drain and adds alkali mouth，It is additionally provided with one for the circulation discharging pump to glycerin treatment tank recycle feed，The entrance point of this circulation discharging pump is connected by the bottom of pipeline with glycerin treatment tank，Circulation discharging delivery side of pump end is connected with the sidewall of glycerin treatment tank by pipeline，It is provided with glycerol product outlet on pipeline between circulation discharging delivery side of pump end and glycerin treatment tank；This apparatus structure is simple, and processing speed is fast, it is possible to isolate multiple side-product, improves the productivity effect of enterprise.
Description
Technical field
The present invention relates to the glycerin treatment device used by a kind of chemical industry, a kind of processing means for reclaiming glycerol in biodiesel and processing method thereof.
Background technology
It is known that, the glycerol that biodiesel factory reclaims contains methanol, soap, fatty acid, methyl ester and small part neutral oil and small part salt etc., must thoroughly process and can sell the purest glycerol, at present, chemical industry is not designed to ripe glycerin treatment device, therefore, market is badly in need of wanting a kind of simple in construction, treatment effeciency high for reclaiming the processing means of glycerol in biodiesel.
Summary of the invention
It is an object of the invention to the deficiency for solving above-mentioned technical problem, it is provided that a kind of processing means for reclaiming glycerol in biodiesel and processing method thereof, this apparatus structure is simple, and processing speed is fast, it is possible to isolate multiple side-product, improves the productivity effect of enterprise.
nullThe present invention solves the deficiency of above-mentioned technical problem，Be the technical scheme is that a kind of for reclaiming the processing means of glycerol in biodiesel，By reactor、Methanol recovery device and glycerin treatment tank composition，Described reactor is provided with agitator，It is provided with charging aperture at the top of reactor、Acid-adding port、Drain and methanol gas outlet，Methanol gas outlet is tightly connected with methanol recovery device，The outer wall of reactor is provided with the heating mantle for being passed through steam，It is arranged on the discharging opening bottom reactor to be connected with glycerin treatment tank by pipeline，Described glycerin treatment tank is provided with drain and adds alkali mouth，It is additionally provided with one for the circulation discharging pump to glycerin treatment tank recycle feed，The entrance point of this circulation discharging pump is connected by the bottom of pipeline with glycerin treatment tank，Circulation discharging delivery side of pump end is connected with the sidewall of glycerin treatment tank by pipeline，The mixing of material in glycerin treatment tank is realized by circulation discharging pump，It is provided with glycerol product outlet on pipeline between circulation discharging delivery side of pump end and glycerin treatment tank；
Described methanol recovery device is made up of multiple condensers and vacuum generator, and multiple condensers are connected in series, and the end at condenser connects vacuum generator, makes methanol gas become liquids recovery after flowing through each condenser successively by opening vacuum generator.
Optimizing further, described reactor is enamel reaction still.
Optimizing further, the pipeline being connected with circulation discharging delivery side of pump end is along the inner chamber being tangentially communicated in glycerin treatment tank of glycerin treatment pot sidewall.
Optimizing further, the bottom of described glycerin treatment tank is additionally provided with sample tap.
A kind of for reclaiming the processing method of the processing means of glycerol in biodiesel, comprise the following steps:
Step one, the glycerol mixture of biodiesel factory initial gross separation is sent into reactor, after start to reactor heat, stir simultaneously, when temperature is raised to 60 DEG C, open methanol gas outlet, and make methanol gas outlet be linked into methanol recovery device, reclaim methanol, when temperature is raised to 80 DEG C, open vacuum generator, reclaiming residue methanol gas by suction function, methanol gas is by collecting after the condenser of series connection；
After step 2, step one process, continue reactor is heated, keep temperature of reaction kettle 80 90 DEG C, in reactor, add hydrochloric acid regulation pH value 34, rear continuous stirring 25 35 minutes, rear standing 1 1.5 hours, soap in glycerol is quickly converted to oil product, and swims in liquid upper, glycerol and salt settling to bottom with methyl ester in glycerol and neutral oil, by pump, the mixture of lower floor's glycerol and salt is squeezed into glycerin treatment tank, standby；
Step 3, by outside circulation discharging pump, the liquid in glycerin treatment tank is circulated flowing, in glycerin treatment tank, add sodium hydroxide simultaneously, adjust the pH value 67 of glycerin treatment pot liquid, the mixture of glycerol and salt carries out gravity settling separation in glycerin treatment tank, top is the glycerol handled well, bottom is the salt after separating, and is disposed, and collects in output glycerol to finished pot.
Liquid level in reactor described in this programme is 75 85%.
The invention has the beneficial effects as follows:
This device, is made up of reactor, methanol recovery device and glycerin treatment tank, simple in construction, and processing speed is fast, can isolate multiple side-product while obtaining glycerol production, improves enterprise's productivity effect；Wherein methanol gas outlet is tightly connected with methanol recovery device, described methanol recovery device is made up of multiple condensers and vacuum generator, multiple condensers are connected in series, end at condenser connects vacuum generator, make methanol gas become liquids recovery after flowing through each condenser successively by opening vacuum generator, when the Methanol Recovery later stage, vacuum valve can be opened, quickly collecting the residue methanol gas in reactor, production efficiency is greatly improved；Secondly, it is additionally provided with circulation discharging pump in the side of glycerin treatment tank, the entrance point of this circulation discharging pump is connected by the bottom of pipeline with glycerin treatment tank, circulation discharging delivery side of pump end is connected with the sidewall of glycerin treatment tank by pipeline, the mixing of material in glycerin treatment tank is realized by circulation discharging pump, it is provided with glycerol product outlet on pipeline between circulation discharging delivery side of pump end and glycerin treatment tank, especially, it should be noted that and circulate pipeline that discharging delivery side of pump end the is connected inner chamber being tangentially communicated in glycerin treatment tank along glycerin treatment pot sidewall, ensure the liquid inwall rotation along process tank of conveying, it is effectively improved the mixing of various materials in process tank, thus save the plenty of time to follow-up process.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention.
Labelling in figure: 1, reactor, 101, charging aperture, 102, acid-adding port, 103, drain, 104, methanol gas outlet, 2, methanol recovery device, 201, condenser, 2011, condensing water inlet, 2012, condensation-water drain, 202, vacuum generator, 3, glycerin treatment tank, 301, drain, 302, add alkali mouth, 303, circulation discharging pump, 304, glycerol product outlet, 305, sample tap, 4, agitator, 5, heating mantle, 501, steam inlet, 502, condensation-water drain.
Detailed description of the invention
Elaborating embodiments of the invention below in conjunction with the accompanying drawings, the present embodiment, premised on technical solution of the present invention, gives detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
nullAs shown in the figure，A kind of for reclaiming the processing means of glycerol in biodiesel，By reactor 1、Methanol recovery device 2 and glycerin treatment tank 3 form，Described reactor 1 is provided with agitator 4，The stirring of material in reactor is realized by agitator 4，It is provided with charging aperture 101 at the top of reactor 1、Acid-adding port 102、Drain 103 and methanol gas outlet 104，Methanol gas outlet 104 and methanol recovery device 2 are tightly connected the recovery realizing methanol gas，The outer wall of reactor 1 is provided with the heating mantle 5 for being passed through steam，The side of heating mantle is provided with steam inlet 501，Opposite side is provided with condensation-water drain 502，The heating to material in reactor is realized by being passed through steam to heating mantle，It is arranged on the discharging opening bottom reactor 1 to be connected with glycerin treatment tank 3 by pipeline，This pipeline is provided with pump，Material bottom reactor is delivered in glycerin treatment tank 3 by pump output power，Described glycerin treatment tank 3 is provided with drain 301 and adds alkali mouth 302，It is additionally provided with one for the circulation discharging pump 303 to glycerin treatment tank recycle feed，The entrance point of this circulation discharging pump 303 is connected by the bottom of pipeline with glycerin treatment tank 3，The port of export of circulation discharging pump 303 is connected with the sidewall of glycerin treatment tank 3 by pipeline，The mixing of material in glycerin treatment tank is realized by circulation discharging pump 303，It is provided with glycerol product outlet 304 on pipeline between the port of export and the glycerin treatment tank 3 of circulation discharging pump 303；
Described methanol recovery device 2 is made up of multiple condensers 201 and vacuum generator 202, the number that condenser is arranged can rationally be arranged, multiple condensers 201 are connected in series, end at condenser 201 connects vacuum generator 202, methanol gas is made to become liquids recovery after flowing through each condenser 201 successively by opening vacuum generator 202, in order to realize optimal using effect, described condenser is provided with condensing water inlet 2011 and condensation-water drain 2012, in order to maximize raising condensation effect, the flow direction of condensed water is contrary with the flow direction of methanol.
In this programme, described reactor is enamel reaction still.
In order to realize preferable using effect, the pipeline being connected with circulation discharging delivery side of pump end is along the inner chamber being tangentially communicated in glycerin treatment tank of glycerin treatment pot sidewall.
The bottom of glycerin treatment tank described in this programme is additionally provided with sample tap, facilitates technical staff's real time sample to detect.
This device can efficiently separate the soap in glycerol, fatty acid methyl ester and small part neutral oil, and salt is got rid of bottom process tank through sedimentation, thus obtains pure glycerol product.
The process step of this processing means is as follows:
Step one, the glycerol mixture of biodiesel factory initial gross separation is sent into reactor, its Liquid level 75 85%, after start to reactor heat, stir simultaneously, when temperature is raised to 60 DEG C, open methanol gas outlet, and make methanol gas outlet be linked into methanol recovery device, reclaim methanol, when temperature is raised to 80 DEG C, opening vacuum generator, reclaim residue methanol gas by suction function, methanol gas is by collecting after the condenser of series connection；
After step 2, step one process, continue reactor is heated, keep temperature of reaction kettle 80 90 DEG C, in reactor, add hydrochloric acid regulation pH value 34, rear continuous stirring 25 35 minutes, rear standing 1 1.5 hours, soap in glycerol is quickly converted to oil product, and swims in liquid upper, glycerol and salt settling to bottom with methyl ester in glycerol and neutral oil, by pump, the mixture of lower floor's glycerol and salt is squeezed into glycerin treatment tank, standby；
Step 3, by outside circulation discharging pump, the liquid in glycerin treatment tank is circulated flowing, in glycerin treatment tank, add sodium hydroxide simultaneously, adjust the pH value 67 of glycerin treatment pot liquid, the mixture of glycerol and salt carries out gravity settling separation in glycerin treatment tank, top is the glycerol handled well, bottom is the salt after separating, and is disposed, and collects in output glycerol to finished pot.
Embodiment one,
Step one, the glycerol mixture of biodiesel factory initial gross separation is sent into reactor, reactor Liquid level 75%, after start to reactor heat, simultaneously agitator start stirring, when temperature is raised to 60 DEG C, open methanol gas outlet, and make methanol gas outlet be linked into methanol recovery device, reclaim methanol, when temperature is raised to 80 DEG C, opening vacuum generator, reclaim residue methanol gas by suction function, methanol gas is by collecting after the condenser of series connection；
After step 2, step one process, continue reactor is heated, keep temperature of reaction kettle 80 DEG C, in reactor, add hydrochloric acid regulation pH value 3, rear continuous stirring 25 minutes, rear standing 1 hour, soap in glycerol is quickly converted to oil product, and swims in liquid upper, glycerol and salt settling to bottom with methyl ester in glycerol and neutral oil, by pump, the mixture of lower floor's glycerol and salt is squeezed into glycerin treatment tank, standby；
Step 3, by outside circulation discharging pump, the liquid in glycerin treatment tank is circulated flowing, in glycerin treatment tank, add sodium hydroxide simultaneously, adjust the pH value 67 of glycerin treatment pot liquid, the mixture of glycerol and salt carries out gravity settling separation in glycerin treatment tank, top is the glycerol handled well, and bottom is the salt after separating, and can periodically take away bottom process tank, it is disposed, collects in output glycerol to finished pot.
Embodiment two,
Step one, the glycerol mixture of biodiesel factory initial gross separation is sent into reactor, its Liquid level 80%, after start to reactor heat, stir simultaneously, when temperature is raised to 60 DEG C, open methanol gas outlet, and make methanol gas outlet be linked into methanol recovery device, reclaim methanol, when temperature is raised to 80 DEG C, opening vacuum generator, reclaim residue methanol gas by suction function, methanol gas is by collecting after the condenser of series connection；
After step 2, step one process, continue reactor is heated, keep temperature of reaction kettle 85 DEG C, in reactor, add hydrochloric acid regulation pH value 3, rear continuous stirring 30 minutes, rear standing 1.2 hours, soap in glycerol is quickly converted to oil product, and swims in liquid upper, glycerol and salt settling to bottom with methyl ester in glycerol and neutral oil, by pump, the mixture of lower floor's glycerol and salt is squeezed into glycerin treatment tank, standby；
Step 3, by outside circulation discharging pump, the liquid in glycerin treatment tank is circulated flowing, in glycerin treatment tank, add sodium hydroxide simultaneously, adjust the pH value 6 of glycerin treatment pot liquid, the mixture of glycerol and salt carries out gravity settling separation in glycerin treatment tank, top is the glycerol handled well, bottom is the salt after separating, and is disposed, and collects in output glycerol to finished pot.
Embodiment three,
Step one, the glycerol mixture of biodiesel factory initial gross separation is sent into reactor, its Liquid level 85%, after start to reactor heat, stir simultaneously, when temperature is raised to 60 DEG C, open methanol gas outlet, and make methanol gas outlet be linked into methanol recovery device, reclaim methanol, when temperature is raised to 80 DEG C, opening vacuum generator, reclaim residue methanol gas by suction function, methanol gas is by collecting after the condenser of series connection；
After step 2, step one process, continue reactor is heated, keep temperature of reaction kettle 90 DEG C, in reactor, add hydrochloric acid regulation pH value 4, rear continuous stirring 35 minutes, rear standing 1.5 hours, soap in glycerol is quickly converted to oil product, and swims in liquid upper, glycerol and salt settling to bottom with methyl ester in glycerol and neutral oil, by pump, the mixture of lower floor's glycerol and salt is squeezed into glycerin treatment tank, standby；
Step 3, by outside circulation discharging pump, the liquid in glycerin treatment tank is circulated flowing, in glycerin treatment tank, add sodium hydroxide simultaneously, adjust the pH value 7 of glycerin treatment pot liquid, the mixture of glycerol and salt carries out gravity settling separation in glycerin treatment tank, top is the glycerol handled well, bottom is the salt after separating, and is disposed, and collects in output glycerol to finished pot.
It is prior art that this programme does not describes technology in detail.
Claims (4)
- null1. one kind is used for reclaiming the processing means of glycerol in biodiesel，It is characterized in that: by reactor、Methanol recovery device and glycerin treatment tank composition，Described reactor is provided with agitator，It is provided with charging aperture at the top of reactor、Acid-adding port、Drain and methanol gas outlet，Methanol gas outlet is tightly connected with methanol recovery device，The outer wall of reactor is provided with the heating mantle for being passed through steam，It is arranged on the discharging opening bottom reactor to be connected with glycerin treatment tank by pipeline，Described glycerin treatment tank is provided with drain and adds alkali mouth，It is additionally provided with one for the circulation discharging pump to glycerin treatment tank recycle feed，The entrance point of this circulation discharging pump is connected by the bottom of pipeline with glycerin treatment tank，Circulation discharging delivery side of pump end is connected with the sidewall of glycerin treatment tank by pipeline，The mixing of material in glycerin treatment tank is realized by circulation discharging pump，It is provided with glycerol product outlet on pipeline between circulation discharging delivery side of pump end and glycerin treatment tank；Described methanol recovery device is made up of multiple condensers and vacuum generator, and multiple condensers are connected in series, and the end at condenser connects vacuum generator, makes methanol gas become liquids recovery after flowing through each condenser successively by opening vacuum generator；Described reactor is enamel reaction still；The pipeline being connected with circulation discharging delivery side of pump end is along the inner chamber being tangentially communicated in glycerin treatment tank of glycerin treatment pot sidewall.
- It is the most according to claim 1 a kind of for reclaiming the processing means of glycerol in biodiesel, it is characterised in that: the bottom of described glycerin treatment tank is additionally provided with sample tap.
- It is the most according to claim 1 a kind of for reclaiming the processing method of the processing means of glycerol in biodiesel, it is characterised in that: comprise the following steps:Step one, the glycerol mixture of biodiesel factory initial gross separation is sent into reactor, after start to reactor heat, stir simultaneously, when temperature is raised to 60 DEG C, open methanol gas outlet, and make methanol gas outlet be linked into methanol recovery device, reclaim methanol, when temperature is raised to 80 DEG C, open vacuum generator, reclaiming residue methanol gas by suction function, methanol gas is by collecting after the condenser of series connection；After step 2, step one process, continue reactor is heated, keep temperature of reaction kettle 80 90 DEG C, in reactor, add salt acid for adjusting pH value 34, rear continuous stirring 25 35 minutes, rear standing 1 1.5 hours, soap in glycerol is quickly converted to oil product, and swims in liquid upper, glycerol and salt settling to bottom with methyl ester in glycerol and neutral oil, by pump, the mixture of lower floor's glycerol and salt is squeezed into glycerin treatment tank, standby；Step 3, by outside circulation discharging pump, the liquid in glycerin treatment tank is circulated flowing, in glycerin treatment tank, add sodium hydroxide simultaneously, adjust the pH value 67 of glycerin treatment pot liquid, the mixture of glycerol and salt carries out gravity settling separation in glycerin treatment tank, top is the glycerol handled well, bottom is the salt after separating, and is disposed, and collects in output glycerol to finished pot.
- Processing method the most according to claim 3, it is characterised in that: the Liquid level in described reactor is 75 85%.
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| CN201410754698.6A CN104496751B (en) | 2014-12-11 | 2014-12-11 | A kind of processing means for reclaiming glycerol in biodiesel and processing method thereof |
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| US7126032B1 (en) * | 2006-03-23 | 2006-10-24 | Sunoco, Inc. (R&M) | Purification of glycerin |
| CN101003741A (en) * | 2007-01-11 | 2007-07-25 | 张伟明 | Reaction kettle for making biologic diesel oil |
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| CN204325188U (en) * | 2014-12-11 | 2015-05-13 | 平顶山市亿鑫达生物能源有限公司 | A kind for the treatment of unit for reclaiming glycerine in biofuel |
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- 2014-12-11 CN CN201410754698.6A patent/CN104496751B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7126032B1 (en) * | 2006-03-23 | 2006-10-24 | Sunoco, Inc. (R&M) | Purification of glycerin |
| CN101003741A (en) * | 2007-01-11 | 2007-07-25 | 张伟明 | Reaction kettle for making biologic diesel oil |
| CN101265160A (en) * | 2008-04-30 | 2008-09-17 | 上海三瑞高分子材料有限公司 | Method for purifying biological diesel oil byproduct glycerin |
| CN204325188U (en) * | 2014-12-11 | 2015-05-13 | 平顶山市亿鑫达生物能源有限公司 | A kind for the treatment of unit for reclaiming glycerine in biofuel |
Non-Patent Citations (1)
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| 生物柴油副产物——甘油精制工艺优化研究;黄艳芹;《新乡学院学报（自然科学版）》;20120831;第29卷(第4期);329-331 * |
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