CN104447201A - Glycerol production device and glycerol production process - Google Patents

Glycerol production device and glycerol production process Download PDF

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Publication number
CN104447201A
CN104447201A CN201410628046.8A CN201410628046A CN104447201A CN 104447201 A CN104447201 A CN 104447201A CN 201410628046 A CN201410628046 A CN 201410628046A CN 104447201 A CN104447201 A CN 104447201A
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China
Prior art keywords
susceptor
glycerol
glycerol production
condenser
dewatering
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CN201410628046.8A
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CN104447201B (en
Inventor
杨正福
赵永国
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SHANGHAI ZHONGHUA PHARMACEUTICAL NANTONG Co Ltd
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SHANGHAI ZHONGHUA PHARMACEUTICAL NANTONG Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Fats And Perfumes (AREA)

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

Glycerol production equipment and glycerol production technique thereof
Technical field
The present invention relates to a kind of glycerol production equipment.
The invention still further relates to and a kind ofly apply the technique that glycerol production equipment carries out glycerol production.
Background technology
Glycerine, this product is Glycerin, containing C 3h 8o 3must not 95.0% be less than.Glycerine is one of important industrial chemicals, there is excellent dissolving and wettability, in industry widespread uses such as medicine, food, makeup, chemical industry, in raw glycerine, glycerol content is generally at about 70-80%, the removal of impurities of raw glycerine, decolouring and concentrated, to purify be very difficult, originally Boiler Steam heating can not be carried out continuously, and High Temperature High Pressure brings danger.Therefore, need to provide a kind of new technical scheme to solve the problems referred to above.
Summary 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 that the present invention also will solve is to provide a kind of glycerol production technique.Overcome the heating of original boiler and need successional problem.
For solving the problems of the technologies described above, glycerol production equipment of the present invention, it comprises multiple dewatering pan, preheater, distillation tower, multiple susceptor, multiple condenser and multiple finished pot, be connected with transferpump bottom described dewatering pan, described transferpump is connected with preheater by pipeline, be connected with distillation tower top bottom described preheater, the first susceptor is connected bottom described distillation tower, described distillation tower top connects the first condenser, described first condenser is connected with the second condenser, second susceptor and the 3rd susceptor are set bottom described first condenser, described second susceptor is connected with the 3rd susceptor, 4th susceptor is set bottom described second condenser, described second susceptor, 3rd susceptor is connected transferpump with the bottom of the 4th susceptor, this transferpump connecting tube is to finished pot.
Multiple dewatering pan is the first dewatering pan and the second dewatering pan, and the first dewatering pan is connected by pipeline with the top of the second dewatering pan.
Multiple finished pot is the first finished pot and the second finished pot, and described first finished pot is connected by pipeline with the top of the second finished pot.
Glycerol production technique of the present invention, comprises the following steps:
A, load weighted crude product glycerine sucked or squeezes in dewatering pan with in-line pump, dewatering pan heating again, controls kettle temperature at 80 ± 5 DEG C, opens the vacuum and cooling water valve of leading to condenser, start draining when kettle temperature reaches 70 DEG C, insulation vacuumizes dewatering time 3-4 hour;
B, the crude product glycerine after dehydration sent into preheater and carry out pre-heating temperature elevation to 140 DEG C ± 10 DEG C;
C, the glycerine by preheater preheats is entered fractionation in distillation tower again, open the cooling water valve of vacuum and condenser on susceptor, keep vacuum tightness below-0.09 MPa, carry out underpressure distillation again, accepting overhead product temperature is 165 ~ 202 DEG C, and overhead product cools in rearmounted glycerine susceptor through condenser;
D, when after the quantity that susceptor glycerine reaches certain, close susceptor material inlet valve, open emptying valve, open material inlet valve and the vacuum valve of another susceptor simultaneously, start to accept material, two susceptor cross-references, are entered in finished pot by transferpump in time by the overhead product in the susceptor of full material after twice filtration;
The inspection of semifinished product is carried out in e, sampling, filling after the assay was approved;
F, stamp, then pack.
In a step, heat to dewatering pan: the heater switch of opening in advance heat-conducting oil furnace, is set in 280 DEG C ± 10 DEG C by Heating temperature, open and control to lead to the heat-conducting oil heating valve of dewatering pan, finally unlatching heat conduction oil circulating pump heats to dewatering pan.
Beneficial effect of the present invention:
1, energy-conservation: overcoming boiler heating needs successional problem, adopts heat-conducting oil heating to carry out at any time;
2, convenient: to adopt heat-conducting oil heating, can heat and stop at any time;
3, environmental protection: overcome in boiler for producing process, needs to use process water, and waste water source produces atmospheric pollution and waste residue, wastewater problem simultaneously;
4, low cost: adopt heat-conducting oil heating running cost low, only needs suitably to supplement the thermal oil consumed.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Fig. 2 is process flow sheet of the present invention.
1, the first dewatering pan, the 2, second dewatering pan, 3, preheater, 4, distillation tower, the 5, first susceptor, 6, the second susceptor, the 7, the 3rd susceptor, the 8, the 4th susceptor, the 9, first condenser, 10, the second condenser, 11, transferpump, the 12, first finished pot, the 13, second finished pot.
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, and this embodiment, only for explaining the present invention, does not form the restriction to protection scope of the present invention.
 
With reference to figure 1, glycerol production equipment of the present invention, it comprises multiple dewatering pan, preheater 3, distillation tower 4, multiple susceptor, multiple condenser and multiple finished pot, multiple dewatering pan is the first dewatering pan 1 and the second dewatering pan 2, first dewatering pan 1 is connected by pipeline with the top of the second dewatering pan 2, be connected with transferpump 11 bottom dewatering pan, transferpump 11 is connected with preheater 3 by pipeline, be connected with distillation tower 4 top bottom preheater 3, the first susceptor 5 is connected bottom distillation tower 4, distillation tower 4 top connects the first condenser 9, first condenser 9 is connected with the second condenser 10, second susceptor 6 and the 3rd susceptor 7 are set bottom first condenser 9, second susceptor 6 is connected with the 3rd susceptor 7, 4th susceptor 8 is set bottom second condenser 10, second susceptor 6, 3rd susceptor 7 is connected transferpump 11 with the bottom of the 4th susceptor 8, this transferpump 11 connecting tube to the first finished pot 12 and second finished pot 13, first finished pot 12 is connected by pipeline with the top of the second finished pot 13.
Repeatedly adopt heat transfer oil electric heating to heat to dewatering pan, convenient and swift, as long as thermal oil keeps circulation in pipeline, off-set facility storage tank has enough feed supplements (thermal oil) and emptying.Crude product glycerine after dehydration is sent into preheater and carries out pre-heating temperature elevation, glycerine by preheater preheats is entered fractionation in distillation tower again, carry out underpressure distillation, overhead product cools in rearmounted glycerine susceptor through condenser, is entered in finished pot in time by the overhead product in the susceptor of full material by transferpump after twice filtration.Adopt whole plant, glycerol production can be carried out continuously, atmospheric pollution and waste residue, wastewater problem can not be produced; Adopt heat-conducting oil heating running cost low, only need suitably to supplement the thermal oil consumed.
Following examples 1-3 is the technique that application glycerol production equipment carries out glycerol production.
Embodiment 1
As shown in Figure 2, glycerol production technique of the present invention, comprises the following steps:
A, open vacuum pump, open the material inlet valve and vacuum valve or in-line pump switch that lead to dewatering pan, load weighted crude product glycerine is sucked or squeezes in dewatering pan with in-line pump, then the heater switch of heat-conducting oil furnace is opened, Heating temperature is set in 270 DEG C, open and control to lead to the heat-conducting oil heating valve of dewatering pan, open heat conduction oil circulating pump to heat to dewatering pan, control kettle temperature at 75 DEG C, open the vacuum and cooling water valve of leading to condenser, draining is started when kettle temperature reaches 70 DEG C, insulation vacuumizes dewatering time 3 hours, wherein moisture is made to be evaporated to the greatest extent,
B, open and control to lead to charging and the heat-conducting oil heating valve of preheater, opening transferpump and the crude product glycerine after dehydration is sent into preheater carry out pre-heating temperature elevation to 130 DEG C;
C, open and control to lead to charging and the heat-conducting oil heating valve of distillation tower, glycerine by preheater preheats is entered fractionation in distillation tower again, open the cooling water valve of vacuum and condenser on susceptor, keep vacuum tightness below-0.09 MPa, controlling heating thermal oil temperature is 210 DEG C, carry out underpressure distillation, accepting overhead product temperature is 165 DEG C, and overhead product cools in rearmounted glycerine susceptor through condenser;
D, when after the quantity that susceptor glycerine reaches certain, close susceptor material inlet valve, open emptying valve, open material inlet valve and the vacuum valve of another susceptor simultaneously, start to accept material, two susceptor cross-references, are entered in finished pot by transferpump in time by the overhead product in the susceptor of full material after twice filtration;
The inspection of semifinished product is carried out in e, sampling, send racking room filling after qualified: get clean plastics Bottle and bottle cap by batch packaging directive before filling, opens filling machine, by filling for glycerine in clean Plastic Bottle, manually adds a cover;
F, stamp, then pack.
Embodiment 2
As shown in Figure 2, glycerol production technique of the present invention, comprises the following steps:
A, open vacuum pump, open the material inlet valve and vacuum valve or in-line pump switch that lead to dewatering pan, load weighted crude product glycerine is sucked or squeezes in dewatering pan with in-line pump, then the heater switch of heat-conducting oil furnace is opened, Heating temperature is set in 280 DEG C, open and control to lead to the heat-conducting oil heating valve of dewatering pan, open heat conduction oil circulating pump to heat to dewatering pan, control kettle temperature at 80 DEG C, open the vacuum and cooling water valve of leading to condenser, draining is started when kettle temperature reaches 70 DEG C, insulation vacuumizes dewatering time 3.5 hours, wherein moisture is made to be evaporated to the greatest extent,
B, open and control to lead to charging and the heat-conducting oil heating valve of preheater, opening transferpump and the crude product glycerine after dehydration is sent into preheater carry out pre-heating temperature elevation to 140 DEG C;
C, open and control to lead to charging and the heat-conducting oil heating valve of distillation tower, glycerine by preheater preheats is entered fractionation in distillation tower again, open the cooling water valve of vacuum and condenser on susceptor, keep vacuum tightness below-0.09 MPa, controlling heating thermal oil temperature is 220 DEG C, carry out underpressure distillation, accepting overhead product temperature is 180 DEG C, and overhead product cools in rearmounted glycerine susceptor through condenser;
D, when after the quantity that susceptor glycerine reaches certain, close susceptor material inlet valve, open emptying valve, open material inlet valve and the vacuum valve of another susceptor simultaneously, start to accept material, two susceptor cross-references, are entered in finished pot by transferpump in time by the overhead product in the susceptor of full material after twice filtration;
The inspection of semifinished product is carried out in e, sampling, send racking room filling after qualified: get clean plastics Bottle and bottle cap by batch packaging directive before filling, opens filling machine, by filling for glycerine in clean Plastic Bottle, manually adds a cover;
F, stamp, then pack.
Embodiment 3
As shown in Figure 2, glycerol production technique of the present invention, comprises the following steps:
A, open vacuum pump, open the material inlet valve and vacuum valve or in-line pump switch that lead to dewatering pan, load weighted crude product glycerine is sucked or squeezes in dewatering pan with in-line pump, then the heater switch of heat-conducting oil furnace is opened, Heating temperature is set in 290 DEG C, open and control to lead to the heat-conducting oil heating valve of dewatering pan, open heat conduction oil circulating pump to heat to dewatering pan, control kettle temperature at 85 DEG C, open the vacuum and cooling water valve of leading to condenser, draining is started when kettle temperature reaches 70 DEG C, insulation vacuumizes dewatering time 4 hours, wherein moisture is made to be evaporated to the greatest extent,
B, open and control to lead to charging and the heat-conducting oil heating valve of preheater, opening transferpump and the crude product glycerine after dehydration is sent into preheater carry out pre-heating temperature elevation to 150 DEG C;
C, open and control to lead to charging and the heat-conducting oil heating valve of distillation tower, glycerine by preheater preheats is entered fractionation in distillation tower again, open the cooling water valve of vacuum and condenser on susceptor, keep vacuum tightness below-0.09 MPa, controlling heating thermal oil temperature is 230 DEG C, carry out underpressure distillation, accepting overhead product temperature is 202 DEG C, and overhead product cools in rearmounted glycerine susceptor through condenser;
D, when after the quantity that susceptor glycerine reaches certain, close susceptor material inlet valve, open emptying valve, open material inlet valve and the vacuum valve of another susceptor simultaneously, start to accept material, two susceptor cross-references, are entered in finished pot by transferpump in time by the overhead product in the susceptor of full material after twice filtration;
The inspection of semifinished product is carried out in e, sampling, send racking room filling after qualified: get clean plastics Bottle and bottle cap by batch packaging directive before filling, opens filling machine, by filling for glycerine in clean Plastic Bottle, manually adds a cover;
F, stamp, then pack.
In a step, start draining when kettle temperature reaches 70 DEG C, insulation vacuumizes dewatering time 3-4 hour, during dehydration, the water in crude product glycerine is eliminated as far as possible, otherwise can evaporate with glycerine, finished product glycerol content is declined.
In step c, controlling heating thermal oil temperature is 220 ± 10 DEG C, and carry out underpressure distillation, during distillation, thermal oil temperature can not be too high, otherwise glycerine can dewater and becomes propenal.
In step e, the inspection of semifinished product is qualified can be filling, within time filling every 2 hours, checks a loading amount, require that loading amount meets intermediates quality standard.
The refining glycerine finally made should be sealed in basin, kept dry, and within three days, planted agent completes filling.
The present invention repeatedly adopts heat transfer oil electric heating, convenient and swift, as long as thermal oil keeps circulation in pipeline, off-set facility storage tank has enough feed supplements (thermal oil) and emptying.And originally adopted steam heating, overcome use steam heating, need configuration boiler and special post operation work (needing through professional training, can be on duty after obtaining card), solve the danger that High Temperature High Pressure is brought simultaneously.
In glycerol production technique of the present invention, adopt heat-conducting oil heating to carry out at any time, overcoming boiler heating needs successional problem; Adopt heat-conducting oil heating, can heat and stop at any time; Overcome in boiler for producing process, need to use process water, waste water source produces atmospheric pollution and waste residue, wastewater problem simultaneously; Adopt heat-conducting oil heating running cost low, only need suitably to supplement the thermal oil consumed.

Claims (5)

1. glycerol production equipment, it is characterized in that: it comprises multiple dewatering pan, preheater, distillation tower, multiple susceptor, multiple condenser and multiple finished pot, be connected with transferpump bottom described dewatering pan, described transferpump is connected with preheater by pipeline, be connected with distillation tower top bottom described preheater, the first susceptor is connected bottom described distillation tower, described distillation tower top connects the first condenser, described first condenser is connected with the second condenser, second susceptor and the 3rd susceptor are set bottom described first condenser, described second susceptor is connected with the 3rd susceptor, 4th susceptor is set bottom described second condenser, described second susceptor, 3rd susceptor is connected transferpump with the bottom of the 4th susceptor, this transferpump connecting tube is to finished pot.
2. glycerol production equipment according to claim 1, is characterized in that: multiple dewatering pan is the first dewatering pan and the second dewatering pan, and the first dewatering pan is connected by pipeline with the top of the second dewatering pan.
3. glycerol production equipment according to claim 1, is characterized in that: multiple finished pot is the first finished pot and the second finished pot, and described first finished pot is connected by pipeline with the top of the second finished pot.
4. application glycerol production equipment according to claim 1 carries out the technique of glycerol production, it is characterized in that, comprises the following steps:
A, load weighted crude product glycerine sucked or squeezes in dewatering pan with in-line pump, dewatering pan heating again, controls kettle temperature at 80 ± 5 DEG C, opens the vacuum and cooling water valve of leading to condenser, start draining when kettle temperature reaches 70 DEG C, insulation vacuumizes dewatering time 3-4 hour;
B, the crude product glycerine after dehydration sent into preheater and carry out pre-heating temperature elevation to 140 DEG C ± 10 DEG C;
C, the glycerine by preheater preheats is entered fractionation in distillation tower again, open the cooling water valve of vacuum and condenser on susceptor, keep vacuum tightness below-0.09 MPa, carry out underpressure distillation again, accepting overhead product temperature is 165 ~ 202 DEG C, and overhead product cools in rearmounted glycerine susceptor through condenser;
D, when after the quantity that susceptor glycerine reaches certain, close susceptor material inlet valve, open emptying valve, open material inlet valve and the vacuum valve of another susceptor simultaneously, start to accept material, two susceptor cross-references, are entered in finished pot by transferpump in time by the overhead product in the susceptor of full material after twice filtration;
The inspection of semifinished product is carried out in e, sampling, filling after the assay was approved;
F, stamp, then pack.
5. application glycerol production equipment according to claim 4 carries out the technique of glycerol production, it is characterized in that: in a step, heat to dewatering pan: the heater switch of opening heat-conducting oil furnace in advance, Heating temperature is set in 280 DEG C ± 10 DEG C, open and control to lead to the heat-conducting oil heating valve of dewatering pan, finally opening heat conduction oil circulating pump and heat to dewatering pan.
CN201410628046.8A 2014-11-11 2014-11-11 Glycerol production device and glycerol production process Active CN104447201B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109293476A (en) * 2018-11-29 2019-02-01 浙江工业大学 Glycerol separating technology and device in a kind of glycerine esterification production waste water

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01250331A (en) * 1988-03-31 1989-10-05 Nippon Oil & Fats Co Ltd Method for purifying glycerol
CN101475444A (en) * 2009-01-22 2009-07-08 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

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01250331A (en) * 1988-03-31 1989-10-05 Nippon Oil & Fats Co Ltd Method for purifying glycerol
CN101475444A (en) * 2009-01-22 2009-07-08 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

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109293476A (en) * 2018-11-29 2019-02-01 浙江工业大学 Glycerol separating technology and device in a kind of glycerine esterification production waste water

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