CN104447201B - Glycerol production device and glycerol production process - Google Patents
Glycerol production device and glycerol production process Download PDFInfo
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- CN104447201B CN104447201B CN201410628046.8A CN201410628046A CN104447201B CN 104447201 B CN104447201 B CN 104447201B CN 201410628046 A CN201410628046 A CN 201410628046A CN 104447201 B CN104447201 B CN 104447201B
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- recipient
- glycerol
- glycerol production
- dewatering
- condenser
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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
Abstract
The invention discloses a glycerol production device. The glycerol production device comprises a plurality of dehydration pots, a preheater, a distillation tower, a plurality of receptors, a plurality of condensers and a plurality of finished product tanks. The invention also discloses a glycerol production process. The glycerol production process comprises the following steps: adding weighed crude glycerol into the dehydration pots, heating the dehydration pots, and starting draining when the temperatures in the pots reach 70 DEG C; adding the dehydrated crude glycerol into the preheater to preheat and increase the temperatures; feeding the glycerol preheated by the preheater into the distillation tower for distilling, then carrying out reduced pressure distillation, cooling the distillation by the condensers, and putting the cooled distillation in glycerol receptors; after the glycerol in the receptors is accumulated to certain amount, by alternately using the two receptors, feeding the distillation after twice of filtering in the full receptors to the finished tanks by a conveying pump in time. According to the glycerol production device, a whole set of device is adopted, so that the glycerol production can be carried out continuously. According to the glycerol production process, heat conduction oil is used for heating the glycerol at any time; the glycerol can be heated and stopped at any time; the glycerol production device and the glycerol production process are low in pollution and low in operation cost.
Description
Technical field
The present invention relates to a kind of glycerol production equipment.
The invention further relates to the technique that a kind of application glycerol production equipment carries out glycerol production.
Background technology
Glycerine, this product is Glycerin, containing C3H8O395.0% must not be less than.Glycerine be important industrial chemicals it
One, with excellent dissolving and wettability, extensively apply in industries such as medicine, food, cosmetics, chemical industry, it is sweet in crude glycerine
Typically in 70-80% or so, removal of impurities, decolouring and the concentration of crude glycerine, purification are extremely difficult to oil content, and originally boiler steams
Vapour heating can not be carried out continuously, and HTHP brings danger.Accordingly, it is desirable to provide a kind of new technical scheme is come on solving
State problem.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of glycerol production equipment.
The technical problem also to be solved of the invention is to provide a kind of glycerol production technique.Original boiler heating is overcome to need to connect
The problem of continuous property.
For solution above-mentioned technical problem, the glycerol production equipment of the present invention, it includes multiple dewatering pans, preheater, distillation
Tower, multiple recipients, multiple condensers and multiple finished pots, the dehydration pot bottom is connected with delivery pump, and the delivery pump leads to
Piping is connected with preheater, and the preheater bottom is connected with destilling tower top, and distillation tower bottom connection first receives
Device, the first condenser of the destilling tower top connection, first condenser and the second condenser connect, first condenser
Bottom arranges the second recipient and the 3rd recipient, and second recipient and the 3rd recipient connect, second condenser
Bottom arranges the 4th recipient, and the bottom of second recipient, the 3rd recipient and the 4th recipient connects delivery pump, and this is defeated
Pump connecting pipe is sent to finished pot.
Multiple dewatering pans pass through pipe for the top of the first dewatering pan and the second dewatering pan, the first dewatering pan and the second dewatering pan
Road connects.
Multiple finished pots lead to for the top of the first finished pot and the second finished pot, first finished pot and the second finished pot
Piping connects.
The glycerol production technique of the present invention, comprises the following steps:
A, squeezed into the suction of load weighted crude product glycerine dewatering pan in or with pipeline pump, then dewatering pan heating, in control pot
At 80 ± 5 DEG C, opening leads to the vacuum and cooling water valve of condenser to temperature, and when kettle temperature reaches 70 DEG C draining is started,
Insulation vacuumizes dewatering time 3-4 hours;
B, by after dehydration crude product glycerine send into preheater carry out pre-heating temperature elevation to 140 DEG C ± 10 DEG C;
C, the glycerine preheated by preheater is entered back in destilling tower it is fractionated, opens vacuum and condenser on recipient
Cooling water valve, keeps vacuum below -0.09 MPa, then carries out vacuum distillation, receives distillate temperature for 165 ~ 202
DEG C, the condensed device of distillate is cooled down in rearmounted glycerine recipient;
D, after recipient glycerine reaches certain quantity, close recipient material inlet valve, open emptying valve, while beating
The material inlet valve and vacuum valve of another recipient are opened, starts to receive material, two recipient cross-references, by the recipient of full material
Interior distillate is entered in finished pot in time by delivery pump after filtering twice;
E, sampling carry out the inspection of semifinished product, filling after the assay was approved;
F, stamp, then pack.
In a steps, dewatering pan heating is given:The heater switch of heat-conducting oil furnace is opened in advance, and heating-up temperature is set in into 280 DEG C
± 10 DEG C, the heat-conducting oil heating valve for leading to dewatering pan is opened and controlled, finally open heat conduction oil circulating pump and heat to dewatering pan.
Beneficial effects of the present invention:
1st, energy-conservation:Overcome boiler heating to need successional problem, can be carried out at any time using heat-conducting oil heating;
2nd, it is convenient:Using heat-conducting oil heating, can heat at any time and stop;
3rd, environmental protection:During overcoming boiler for producing, need to use water for industrial use, waste water source produce simultaneously air pollution and
Waste residue, wastewater problem;
4th, low cost:It is low using heat-conducting oil heating operating cost, it is only necessary to appropriate to supplement the conduction oil for consuming.
Description of the drawings
Fig. 1 is the structural representation of the present invention.
Fig. 2 is the process chart of the present invention.
1st, the first dewatering pan, the 2, second dewatering pan, 3, preheater, 4, destilling tower, the 5, first recipient, 6, second receives
Device, the 7, the 3rd recipient, the 8, the 4th recipient, the 9, first condenser, the 10, second condenser, 11, delivery pump, the 12, first finished product
Tank, the 13, second finished pot.
Specific embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment and accompanying drawing, the invention will be further described, should
Embodiment is only used for the explanation present invention, does not constitute the restriction to protection scope of the present invention.
With reference to Fig. 1, the glycerol production equipment of the present invention, it includes multiple dewatering pans, preheater 3, destilling tower 4, Duo Gejie
Receiver, multiple condensers and multiple finished pots, multiple dewatering pans are the first dewatering pan 1 and the second dewatering pan 2, the first dewatering pan 1
Connected by pipeline with the top of the second dewatering pan 2, dehydration pot bottom is connected with delivery pump 11, delivery pump 11 pass through pipeline with it is pre-
Hot device 3 connects, and the bottom of preheater 3 is connected with the top of destilling tower 4, and the bottom of destilling tower 4 connects the first recipient 5, the top of destilling tower 4
Connect the first condenser 9, the first condenser 9 and the second condenser 10 connect, the bottom of the first condenser 9 arranges the second recipient 6
With the 3rd recipient 7, the second recipient 6 and the 3rd recipient 7 connect, and the bottom of the second condenser 10 arranges the 4th recipient 8, the
The bottom connection delivery pump 11 of two recipients 6, the 3rd recipient 7 and the 4th recipient 8, the connecting pipe of delivery pump 11 to first
The top of the finished pot 13 of finished pot 12 and second, the first finished pot 12 and the second finished pot 13 is connected by pipeline.
Heat transfer oil electric heating is employed many times to heat to dewatering pan, it is convenient and swift, it is auxiliary as long as conduction oil keeps circulation in pipeline
Facility storage tank is helped there are enough feed supplements(Conduction oil)With emptying.Crude product glycerine after dehydration is sent into into preheater to be preheated
Heat up, the glycerine preheated by preheater is entered back in destilling tower and is fractionated, carry out vacuum distillation, the condensed device cooling of distillate
In rearmounted glycerine recipient, the distillate in the recipient of full material is entered into finished product by delivery pump after filtering twice in time
In tank.Using complete equipment so that glycerol production can be carried out continuously, air pollution and waste residue, wastewater problem will not be produced;Adopt
It is low with heat-conducting oil heating operating cost, it is only necessary to appropriate to supplement the conduction oil for consuming.
Example 1 below -3 is the technique for carrying out glycerol production using glycerol production equipment.
Embodiment 1
As shown in Fig. 2 the glycerol production technique of the present invention, comprises the following steps:
A, unlatching vavuum pump, opening is led to the material inlet valve and vacuum valve or pipeline switch pump of dewatering pan, will be weighed
Crude product glycerine suction or squeezed in dewatering pan with pipeline pump, be then turned on the heater switch of heat-conducting oil furnace, heating-up temperature is set
270 DEG C are scheduled on, the heat-conducting oil heating valve for leading to dewatering pan is opened and control, heat conduction oil circulating pump are opened and is heated to dewatering pan,
At 75 DEG C, opening leads to the vacuum and cooling water valve of condenser to control kettle temperature, starts when kettle temperature reaches 70 DEG C
Draining, insulation vacuumizes dewatering time 3 hours so as to which middle moisture evaporation is to the greatest extent;
B, the charging of preheater and heat-conducting oil heating valve are opened and control to lead to, open delivery pump by the crude product after dehydration
Glycerine sends into preheater and carries out pre-heating temperature elevation to 130 DEG C;
C, open and control to lead to the charging of destilling tower and heat-conducting oil heating valve, by the glycerine preheated by preheater again
Into in destilling tower be fractionated, open recipient on vacuum and condenser cooling water valve, keep vacuum -0.09 MPa with
Under, it is 210 DEG C to control to heat heat conduction oil temperature, carries out vacuum distillation, receives distillate temperature for 165 DEG C, and distillate is condensed
Device is cooled down in rearmounted glycerine recipient;
D, after recipient glycerine reaches certain quantity, close recipient material inlet valve, open emptying valve, while beating
The material inlet valve and vacuum valve of another recipient are opened, starts to receive material, two recipient cross-references, by the recipient of full material
Interior distillate is entered in finished pot in time by delivery pump after filtering twice;
E, sampling carry out the inspection of semifinished product, it is qualified after send racking room filling:Cleaning is got before filling by batch packaging directive
Plastics Bottle and bottle cap, open bottle placer, by glycerine it is filling cleaning plastic bottle in, manually add a cover;
F, stamp, then pack.
Embodiment 2
As shown in Fig. 2 the glycerol production technique of the present invention, comprises the following steps:
A, unlatching vavuum pump, opening is led to the material inlet valve and vacuum valve or pipeline switch pump of dewatering pan, will be weighed
Crude product glycerine suction or squeezed in dewatering pan with pipeline pump, be then turned on the heater switch of heat-conducting oil furnace, heating-up temperature is set
280 DEG C are scheduled on, the heat-conducting oil heating valve for leading to dewatering pan is opened and control, heat conduction oil circulating pump are opened and is heated to dewatering pan,
At 80 DEG C, opening leads to the vacuum and cooling water valve of condenser to control kettle temperature, starts when kettle temperature reaches 70 DEG C
Draining, insulation vacuumizes dewatering time 3.5 hours so as to which middle moisture evaporation is to the greatest extent;
B, the charging of preheater and heat-conducting oil heating valve are opened and control to lead to, open delivery pump by the crude product after dehydration
Glycerine sends into preheater and carries out pre-heating temperature elevation to 140 DEG C;
C, open and control to lead to the charging of destilling tower and heat-conducting oil heating valve, by the glycerine preheated by preheater again
Into in destilling tower be fractionated, open recipient on vacuum and condenser cooling water valve, keep vacuum -0.09 MPa with
Under, it is 220 DEG C to control to heat heat conduction oil temperature, carries out vacuum distillation, receives distillate temperature for 180 DEG C, and distillate is condensed
Device is cooled down in rearmounted glycerine recipient;
D, after recipient glycerine reaches certain quantity, close recipient material inlet valve, open emptying valve, while beating
The material inlet valve and vacuum valve of another recipient are opened, starts to receive material, two recipient cross-references, by the recipient of full material
Interior distillate is entered in finished pot in time by delivery pump after filtering twice;
E, sampling carry out the inspection of semifinished product, it is qualified after send racking room filling:Cleaning is got before filling by batch packaging directive
Plastics Bottle and bottle cap, open bottle placer, by glycerine it is filling cleaning plastic bottle in, manually add a cover;
F, stamp, then pack.
Embodiment 3
As shown in Fig. 2 the glycerol production technique of the present invention, comprises the following steps:
A, unlatching vavuum pump, opening is led to the material inlet valve and vacuum valve or pipeline switch pump of dewatering pan, will be weighed
Crude product glycerine suction or squeezed in dewatering pan with pipeline pump, be then turned on the heater switch of heat-conducting oil furnace, heating-up temperature is set
290 DEG C are scheduled on, the heat-conducting oil heating valve for leading to dewatering pan is opened and control, heat conduction oil circulating pump are opened and is heated to dewatering pan,
At 85 DEG C, opening leads to the vacuum and cooling water valve of condenser to control kettle temperature, starts when kettle temperature reaches 70 DEG C
Draining, insulation vacuumizes dewatering time 4 hours so as to which middle moisture evaporation is to the greatest extent;
B, the charging of preheater and heat-conducting oil heating valve are opened and control to lead to, open delivery pump by the crude product after dehydration
Glycerine sends into preheater and carries out pre-heating temperature elevation to 150 DEG C;
C, open and control to lead to the charging of destilling tower and heat-conducting oil heating valve, by the glycerine preheated by preheater again
Into in destilling tower be fractionated, open recipient on vacuum and condenser cooling water valve, keep vacuum -0.09 MPa with
Under, it is 230 DEG C to control to heat heat conduction oil temperature, carries out vacuum distillation, receives distillate temperature for 202 DEG C, and distillate is condensed
Device is cooled down in rearmounted glycerine recipient;
D, after recipient glycerine reaches certain quantity, close recipient material inlet valve, open emptying valve, while beating
The material inlet valve and vacuum valve of another recipient are opened, starts to receive material, two recipient cross-references, by the recipient of full material
Interior distillate is entered in finished pot in time by delivery pump after filtering twice;
E, sampling carry out the inspection of semifinished product, it is qualified after send racking room filling:Cleaning is got before filling by batch packaging directive
Plastics Bottle and bottle cap, open bottle placer, by glycerine it is filling cleaning plastic bottle in, manually add a cover;
F, stamp, then pack.
In a steps, draining is started when kettle temperature reaches 70 DEG C, insulation vacuumizes dewatering time 3-4 hours, is dehydrated
When, the water in crude product glycerine is eliminated as far as possible, otherwise can evaporate with glycerine, decline finished product glycerol content.
In step c, it is 220 ± 10 DEG C to control to heat heat conduction oil temperature, carries out vacuum distillation, during distillation, heat conduction oil temperature
Degree can not be too high, and otherwise glycerine can be dehydrated and become methacrylaldehyde.
In step e, the inspection of semifinished product is qualified can be filling, when filling per 2 hours check a loading amount, it is desirable to loading amount accord with
Close intermediate products quality standard.
The refined glycerine being finally made should be sealed in basin, kept dry, and planted agent completes filling within three days.
The present invention is employed many times heat transfer oil electric heating, convenient and swift, as long as conduction oil keeps circulation, auxiliary equipment in pipeline
Storage tank has enough feed supplements(Conduction oil)With emptying.And heated using steam originally, overcome and heated using steam, need to match somebody with somebody
Put boiler and special post operation work(Need through professional training, obtaining can be on duty after card), while solving HTHP band
The danger come.
In the glycerol production technique of the present invention, can at any time be carried out using heat-conducting oil heating, overcome boiler heating to need continuous
The problem of property;Using heat-conducting oil heating, can heat at any time and stop;During overcoming boiler for producing, need using industrial
Water, wastes water source and produces air pollution and waste residue, wastewater problem simultaneously;It is low using heat-conducting oil heating operating cost, it is only necessary to suitable
When the conduction oil for supplementing consumption.
Claims (4)
1. glycerol production equipment, it is characterised in that:It includes multiple dewatering pans, preheater, destilling tower, multiple recipients, multiple
Condenser and multiple finished pots, the dehydration pot bottom is connected with delivery pump, and the delivery pump is connected by pipeline with preheater,
The preheater bottom is connected with destilling tower top, and the distillation tower bottom connects the first recipient, and the destilling tower top connects
The first condenser is connect, first condenser and the second condenser connect, and the first condenser bottom arranges the second recipient
With the 3rd recipient, second recipient and the 3rd recipient connect, and the second condenser bottom arranges the 4th recipient,
The bottom connection delivery pump of second recipient, the 3rd recipient and the 4th recipient, the delivery pump connecting pipe of recipient
To finished pot.
2. glycerol production equipment according to claim 1, it is characterised in that:Multiple dewatering pans are the first dewatering pan and second
The top of dewatering pan, the first dewatering pan and the second dewatering pan is connected by pipeline.
3. glycerol production equipment according to claim 1, it is characterised in that:Multiple finished pots are the first finished pot and second
The top of finished pot, first finished pot and the second finished pot is connected by pipeline.
4. the technique that application glycerol production equipment according to claim 1 carries out glycerol production, it is characterised in that include with
Lower step:
A, squeezed into the suction of load weighted crude product glycerine dewatering pan in or with pipeline pump, the heating that heat-conducting oil furnace is opened in advance is opened
Close, heating-up temperature is set in into 280 DEG C ± 10 DEG C, open and control the heat-conducting oil heating valve for leading to dewatering pan, finally open
Heat conduction oil circulating pump is heated to dewatering pan, and at 80 ± 5 DEG C, opening leads to the vacuum and cooling water valve of condenser to control kettle temperature
Door, draining is started when kettle temperature reaches 70 DEG C, and insulation vacuumizes dewatering time 3-4 hours;
B, by after dehydration crude product glycerine send into preheater carry out pre-heating temperature elevation to 140 DEG C ± 10 DEG C;
C, by the glycerine preheated by preheater enter back in destilling tower be fractionated, open recipient on vacuum and condenser cooling
Penstock, keeps vacuum below -0.09 MPa, then carries out vacuum distillation, receives distillate temperature for 165 ~ 202 DEG C, evaporates
Go out the condensed device of thing to cool down in rearmounted glycerine recipient;
D, after recipient glycerine reaches certain quantity, close recipient material inlet valve, emptying valve is opened, while opening another
The material inlet valve and vacuum valve of one recipient, starts to receive material, two recipient cross-references, by the recipient of full material
Distillate is entered in finished pot in time by delivery pump after filtering twice;
E, sampling carry out the inspection of semifinished product, filling after the assay was approved;
F, stamp, then pack.
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CN201410628046.8A CN104447201B (en) | 2014-11-11 | 2014-11-11 | Glycerol production device and glycerol production process |
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CN201410628046.8A CN104447201B (en) | 2014-11-11 | 2014-11-11 | Glycerol production device and glycerol production process |
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CN104447201A CN104447201A (en) | 2015-03-25 |
CN104447201B true CN104447201B (en) | 2017-05-10 |
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CN109293476B (en) * | 2018-11-29 | 2021-08-10 | 浙江工业大学 | Glycerol separation process and device in glyceride production wastewater |
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Publication number | Priority date | Publication date | Assignee | Title |
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JPH01250331A (en) * | 1988-03-31 | 1989-10-05 | Nippon Oil & Fats Co Ltd | Method for purifying glycerol |
CN101475444B (en) * | 2009-01-22 | 2012-05-30 | 江门市鸿捷精细化工有限公司 | Partial dehydration and purification process for crude glycerine |
CN201426985Y (en) * | 2009-04-25 | 2010-03-24 | 博兴华润油脂化学有限公司 | Novel glycerin distillation device |
CN203916123U (en) * | 2014-07-10 | 2014-11-05 | 南通市康桥油脂有限公司 | A kind of glycerine rectifying distilling apparatus |
CN204310985U (en) * | 2014-11-11 | 2015-05-06 | 上海中华药业南通有限公司 | Glycerol production equipment |
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