CN205550257U - Device of microwave response preparation ethylene glycol antimony - Google Patents
Device of microwave response preparation ethylene glycol antimony Download PDFInfo
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- CN205550257U CN205550257U CN201620362807.4U CN201620362807U CN205550257U CN 205550257 U CN205550257 U CN 205550257U CN 201620362807 U CN201620362807 U CN 201620362807U CN 205550257 U CN205550257 U CN 205550257U
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Abstract
The utility model provides a device of microwave response preparation ethylene glycol antimony, includes microwave reation kettle, microwave reation kettle comprises the cauldron body, microwave heating equipment, agitating unit, charge door, condensing reflux device, apron, discharge valve, heat preservation and temperature measuring device, it is external that microwave heating equipment is located the cauldron, agitating unit is arranged in the cauldron body to link to each other with the apron, the apron is located the cauldron body and goes up with the seal pot body, the charge door is located the apron, and is furnished with the lid, the discharge valve is located cauldron body lower extreme, the heat preservation is located cauldron body below, the condensing reflux unit bit is on the apron to with cauldron body intercommunication, the water that is used for the discharge reaction to generate, temperature measuring device installs the exit end at the condensing reflux device. Utilize the utility model discloses preparation ethylene glycol antimony, it is fast to have a rate of heating, and reaction time is short, and the conversion rate is high, and the straight yield of final products is high, and the productivity is big, advantage such as with low costs.
Description
Technical field
This utility model preparation relates to the preparation facilities of a kind of antimony glycol, is specifically related to a kind of microwave reaction and prepares second two
The device of alcohol antimony.
Background technology
Antimony glycol, chemical molecular formula is Sb2(OCH2CH2O)3, relative molecular weight is 423.66, and theoretical antimony content is
57.5%, it is a kind of new catalyst in polyethylene terephthalate (PET) polycondensation process.Owing to catalytic effect is excellent,
Therefore, antimony oxide, the upgraded product of antimony acetate during antimony glycol has become the antimony-based catalyst of polyester catalytic process.
In antimony glycol production technology, ethylene glycol and antimony oxide the reaction synthesizing antimony glycol is whole technique
During critical process.The speed of synthetic reaction process directly affects the speed of whole production process, the most directly concerns equipment
Investment, place size and yield.The building-up process of existing antimony glycol all uses the steam heating of routine, electrical heating side
Formula, thus, the response time is long.
The preparation method of a kind of antimony glycol disclosed in CN103044200B, the method is by antimony oxide and ethylene glycol
Put in closed reactor for 1:4～7 in mass ratio, under pressure is-0.05～-0.07MPa, be heated to 120 with steam
～150 DEG C react 1～3 hour.The method response time is long, simultaneously need to carry out under a vacuum.
CN1120854C discloses the preparation method of a kind of glycol antimony catalyst for polyester, and the method is by three oxidations two
Antimony and ethylene glycol are by weight for antimony oxide: ethylene glycol=1:2.5～4, conventional heating 140～160 DEG C, and backflow is anti-
Answer 4～6 hours.This method is under the effect not having vacuum, and the response time needs 4～6 hours.
Use conventional heating mode synthesizing glycol antimony, or the response time is long, or need to react under vacuo, this
Sample, energy consumption is high, is unfavorable for improving productivity simultaneously.
Utility model content
Technical problem to be solved in the utility model is, there is time length, energy consumption height for the synthesis of existing antimony glycol
Defect, it is provided that the microwave reaction that a kind of energy consumption is low, the response time is short prepares the device of antimony glycol.
This utility model solves its technical problem and be the technical scheme is that a kind of microwave reaction prepares antimony glycol
Device, including microwave reaction kettle, described microwave reaction kettle is returned by kettle, microwave heating equipment, agitating device, charge door, condensation
Stream device, cover plate, discharge valve, heat-insulation layer and temperature measuring equipment composition, described microwave heating equipment is positioned at outside kettle, described stirring dress
Setting in kettle, and being connected with cover plate, described cover plate is positioned on kettle to seal kettle, and described charge door is positioned on cover plate,
And it is furnished with lid, described discharge valve is positioned at kettle lower end, and described heat-insulation layer is positioned at below kettle, and described condensation reflux unit is positioned at
On cover plate, and connecting with kettle, for discharging the water that reaction generates, described temperature measuring equipment is arranged on the outlet of condensation reflux unit
End.
Further, also include microwave distillation still, described microwave distillation still by kettle, microwave heating equipment, agitating device, add
Material mouth, condensing unit, cover plate, discharge valve, heat-insulation layer and temperature measuring equipment composition, described microwave heating equipment is positioned at outside kettle, institute
Stating agitating device to be positioned in kettle, and be connected with cover plate, described cover plate is positioned on kettle to seal kettle, and described charge door is positioned at
On cover plate, and being furnished with lid, described discharge valve is positioned at kettle lower end, and described heat-insulation layer is positioned at below kettle, described condensing unit
Being positioned on cover plate, and connect with kettle, be used for reclaiming ethylene glycol, described temperature measuring equipment is arranged on the entrance point of condensing unit.
Material used by kettle is not absorb or seldom absorb the nonmetallic substance of microwave, generally uses heat resistant glass, as
Silica glass, devitrified glass, high-boron-silicon glass, pottery, temperature resistant plastic, such as politef, heatproof fiberglass.Absorb micro-
The material of ripple such as graphite, can not.Because owing to graphite is easiest to absorb microwave and produce high temperature, making ethylene glycol and antimony oxide
Mixture heats up.This intensification, as popular response heats, it is impossible to make ethylene glycol dipole molecule high frequency strenuous exercise and collision,
Thus can not fully be fully contacted with antimony oxide molecule, synthetic reaction can not quickly be carried out.
Kettle is more suitable with cylinder, and kettle size is determined as required.
Cover plate is used for sealing kettle, and its material can be identical with kettle, it would however also be possible to employ the materials such as rustless steel.
Microwave heating equipment, can carry out being evenly arranged microwave tube to use annulus or tetragonal body form, make microwave uniform
In kettle outer surface.The size of microwave power, is arranged according to kettle size, to fully ensure that the temperature needed for reaction.Micro-
Wave frequency is conventional frequency 915MHz or 2450MHz of industry heating.
Agitating device is that driven by motor shaft rotates.Power of motor according to kettle volume it needs to be determined that.Anchor formula is used to stir
Mix is fitted, and mixing speed is generally 30-100 rev/min.Shaft uses rustless steel or stainless steel with material contact portion
Matter appearance parcel temperature resistant plastic is made.
The size of charge door determines, depending on kettle volume size.Typically it is as the criterion meeting the needs of feeding quantity.And join
There is lid, after adding material, seal lid.
Condensation reflux unit is water condensing tube, is furnished with thermometer or temperature indicator device, and water condenser is furnished with turnover
The mouth of a river, and it is respectively provided with valve, it is used for controlling exit gas temperature.
Discharge valve is used for blowing.Size determines according to kettle volume.The form of discharge valve uses in prior art and to close most
Suitable mode is carried out.
Heat-insulation layer is for the insulation of kettle material.
The structure of microwave distillation still is essentially identical with the structure of microwave reaction kettle, and except for the difference that condensing unit is different, reaction
The condensing unit of tank is for discharging the water that reaction generates, and the condensing unit of alembic is used for reclaiming ethylene glycol.
The vapo(u)rizing temperature of microwave distillation still controls at 120～195 DEG C, and the ethylene glycol return collecting fraction during this period of time makes
With.Using microwave distillation mother solution, speed is fast, because ethylene glycol easily absorbs microwave, heating is fast, and evaporation is also fast, is by tradition equally
Mode of heating can not than.
Utilize said apparatus to carry out the method that microwave reaction prepares antimony glycol, comprise the following steps:
(1) it is synthesized
By raw material antimony oxide with ethylene glycol in the ratio that solid-to-liquid ratio is 1:2～10, the unit of ratio is g/mL or kg/
L, put into microwave heating equipment, condensation reflux unit, agitator microwave reaction kettle in, start microwave heating equipment, control
Reaction temperature processed is 140～190 DEG C, and the response time is 15～55 minutes, and the temperature controlling condensation reflux unit exit gas is
90～120 DEG C；
(2) remove impurity decolouring
Adding activated carbon in reacted antimony glycol hot solution, the addition of activated carbon is aoxidized by 5～15kg/ tons three
Two antimony are carried out, and insulated and stirred (mixing time preferably 10～12 minutes) carries out remove impurity of decolouring, and then filters, the second after filtration
The temperature of glycol antimony solution controls at 110～140 DEG C；
(3) crystallisation by cooling
Ethylene glycol antimony solution after filtering is put into and is controlled chilling temperature under crystallizer, stirring, allow antimony glycol by
Slowly separate out during step cooling, after chilling temperature arrives room temperature, be filtrated to get wet ethylene glycol antimony and ethylene glycol mother solution；
(4) it is dried
The wet ethylene glycol antimony of gained is dried, obtains antimony glycol product；
(5) mother solution distillation
The ethylene glycol mother solution of gained is joined in the microwave distillation still with microwave heating equipment, with microwave heating, steams
Going out ethylene glycol, bottoms reclaim.
Further, in step (3), described in be filtered into centrifuge filter.
Further, in step (5), controlling distillation outlet temperature is 120～195 DEG C.
Microwave is a kind of electromagnetic wave, its frequency at 300MHz～300GHz, corresponding wave-length coverage be 1mm～
1000mm.The conventional frequency of industry heating is 915MHz and 2450MHz.Microwave it be high by heated object internal dipole molecule
Frequently strenuous exercise, produces " internal friction heat " and makes heated temperature of charge raise, be not necessary to any heat transfer process, just can make material
Heating simultaneously, heat up simultaneously in inside and outside, firing rate is fast and uniform, it is only necessary to the part or several of the energy consumption of traditional heating mode
Ten/once can reach heating purpose.Microwave heating is quick, is overall heating simultaneously.
Ethylene glycol is polar organic solvent, and its dielectric constant is 41.2(20 DEG C).After ethylene glycol absorbs microwave, ethylene glycol
Dipole molecule carries out strenuous exercise with frequency 915MHz or 2450MHz.Strenuous exercise both produced heat energy, has made solution quickly rise
Temperature, too increases the quickly diffusion of glycol molecule and the sharp impacts with antimony oxide, is greatly accelerated antimony oxide
Speed with glycol reaction.The possible cause being greatly improved antimony oxide and glycol reaction speed is that microwave causes second
H, O group in-OH ion in glycol is easily broken off during sharp impacts, and the H atom of fracture is divided with antimony oxide
O atom in son combines and generates hydrone H2Each glycol molecule of O(sloughs 2 hydrogen atoms, divides with an antimony oxide
An oxygen atom in son combines and generates a hydrone), thus accelerate response speed, and then reaction is raw within the unit interval
Become more antimony glycol, this reaction to achieve employing conventional heating mode to be beyond one's reach effect.It is specifically shown in three oxidations two
Antimony and glycol reaction formula.
Antimony oxide and glycol reaction formula:
。
Ethylene glycol and antimony oxide, at a temperature of 140～190 DEG C, when the response time is 15～55 minutes, just can fill
Dividing reaction to produce ethylene glycol antimony solution, solution is limpid, only high price antimony, as tetravalence antimony or priceless antimony can not react.Three oxidations
High price antimony in two antimony only has only a few, thus in ethylene glycol antimony solution, precipitate is little.
The outlet temperature of backflow controls at 90～120 DEG C, and ethylene glycol and antimony oxide produce necessarily in synthetic reaction
The water of amount, the moisture of generation needs to separate in time, and otherwise, the antimony glycol of generation can hydrolyze and become ethylene glycol and three oxidations
Two antimony.
The ethylene glycol saturated vapor dividing potential drop of aqueous 0.5% is to be 63.11Pa when 80 DEG C, is 298.35Pa when 90 DEG C, 100 DEG C
Time be 757.84Pa, be 1577.81Pa when 110 DEG C, be 2953.84Pa when 120 DEG C.Control bypass outlet temperature 90～120
DEG C it is that beneficially reaction is normally carried out for the timely sharp separation of moisture that fully will generate in course of reaction, simultaneously as instead
Less than 1 hour between Ying Shi, the amount of the ethylene glycol distilled is little.
Utilize this utility model to prepare antimony glycol, have the advantages that
(1), during utilizing microwave reaction synthesizing glycol antimony, microwave not only provided thermal source but also because ethylene glycol dipole molecule
Absorb microwave strenuous exercise and collision.Microwave heating is the internal heating of material, and speed is fast；Ethylene glycol dipole molecule strenuous exercise,
Considerably increase being fully contacted of ethylene glycol and antimony oxide molecule, be greatly accelerated the speed of synthesizing glycol antimony.Therefore,
This method, firing rate is fast, and the response time is short, and conversion ratio is high, and final products direct yield is high, and production capacity is big, low cost.
(2) energy consumption is low, and in its course of reaction, required energy consumption is the 50% of popular response synthesis, even lower；Because the method
Be synthesized that required time is existing mode of heating 1/2 or 1/3；It is not required to carry out under vacuo；Heating need not boiler and produces
Raw steam, does not has huge steam-supplying system.
(3) needed for synthesizing glycol antimony, site area is little, and one is because reaction need not vacuum system, and two is not have boiler
Air supply system, three is that the response time is short, and production efficiency is high, it is not necessary to more react facility.
(4), under normal pressure, microwave device distillation efficiency is 2～4 times of Conventional espresso device.
Accompanying drawing explanation
Fig. 1 is the structural representation of the microwave reaction kettle of this utility model embodiment；
Fig. 2 is the structural representation of the microwave distillation still of this utility model embodiment.
Detailed description of the invention
Below in conjunction with drawings and Examples, the utility model is described in further detail.
With reference to Fig. 1, the microwave reaction of the present embodiment prepares the device of antimony glycol, including microwave reaction kettle, and described microwave
Reactor is by kettle 1, microwave heating equipment 2, agitating device 3, charge door 4, condensation reflux unit 5, cover plate 6, discharge valve 7, guarantor
Temperature layer 8 and temperature measuring equipment 9 form；Described microwave heating equipment 2 is positioned at outside kettle 1, and described agitating device 3 is positioned in kettle 1, and
Being connected with cover plate 6, described cover plate 6 is positioned on kettle 1 to seal kettle 1, and described charge door 4 is positioned on cover plate 6, and is furnished with lid
Son, described discharge valve 7 is positioned at kettle 1 lower end, and described heat-insulation layer 8 is positioned at below kettle 1, and described condensation reflux unit 5 is positioned at lid
On plate 6, and connecting with kettle 1, for discharging the water that reaction generates, described temperature measuring equipment 9 is arranged on going out of condensation reflux unit 5
Mouth end.
In the present embodiment, described microwave reaction is prepared the device of antimony glycol and is also included microwave distillation still, as in figure 2 it is shown,
Described microwave distillation still is by kettle 1, microwave heating equipment 2, agitating device 3, charge door 4, condensing unit 10, cover plate 6, discharge valve
7, heat-insulation layer 8 and temperature measuring equipment 9 form, and described microwave heating equipment 2 is positioned at outside kettle 1, and described agitating device 3 is positioned at kettle 1
In, and be connected with cover plate 6, described cover plate 6 is positioned on kettle 1 to seal kettle 1, and described charge door 4 is positioned on cover plate 6, and joins
Having lid, described discharge valve 7 to be positioned at kettle 1 lower end, described heat-insulation layer 8 is positioned at below kettle 1, and described condensing unit 10 is positioned at lid
On plate 6, and connecting with kettle 1, be used for reclaiming ethylene glycol, described temperature measuring equipment 9 is arranged on the entrance point of condensing unit 10.
In the present embodiment, described microwave heating equipment 2 uses the form of annulus to carry out being evenly arranged microwave tube, makes microwave equal
Even in kettle outer surface.Certainly, it is possible to use tetragonal body form to carry out being evenly arranged microwave tube.
In the present embodiment, described condensation reflux unit 5 is water condensing tube, and water condensing tube is furnished with intake-outlet, and joins respectively
There is valve, be used for controlling exit gas temperature.
In the present embodiment, described agitating device 3 is anchor agitator.
In the present embodiment, described heat-insulation layer 8 is for the insulation of kettle material.
In the present embodiment, the structure of microwave distillation still is essentially identical with the structure of microwave reaction kettle, except for the difference that condenses dress
Putting difference, the condensing unit of reactor is for discharging the water that reaction generates, and the condensing unit of distillating still is used for reclaiming ethylene glycol.
The work process of described microwave reaction kettle is: first checks whether each several part is installed by Fig. 1 requirement and puts in place, if just
Often.After confirming normally, clean kettle 1 and condensation reflux unit 5, and close discharge valve 7.Then, by dispensing requirements, starting
In the case of agitating device 3, it is sequentially added into ethylene glycol and antimony oxide at charge door 4, after material adds, builds lid.Adding
During material, start microwave heating equipment 2 and heat.Control reaction temperature well.By entering of regulation condensation reflux unit 5
The water yield, reaches to control the temperature in its exit.After reaction reaches the stipulated time, check the material in kettle, confirm limpid with
No.Confirm limpid after, add activated carbon carry out insulation decolouring.Then filter.Filtrate enters crystallisation by cooling.Crystal is wet second two
Alcohol antimony, after filtration, wet ethylene glycol antimony is sent to dry, and mother solution carries out microwave distillation, reclaims ethylene glycol and returns use.
The work process of described microwave distillation still is: first checks whether each several part is installed by Fig. 2 requirement and puts in place, if just
Often.After confirming normally, clean kettle 1 and condensing unit 10, and close discharge valve 7.Then, add at charge door 4 on request
Ethylene glycol mother solution, after material adds, builds lid.During charging, start microwave heating equipment 2 and heat.On request
Control vapo(u)rizing temperature well, by regulating the inflow of condensing unit 10, reach to control the temperature in condensing unit exit.See at any time
Examine the inventory in distillating still.Ethylene glycol mother solution is added in time by charge door 4.When only solid residue in distillating still timely
Close the power supply of microwave heating equipment.Ethylene glycol after distillation returns and uses.Residue after distillating still clears in time, by rule
Surely gather.Cleaning gets out distillating still, for next time.
The antimony oxide that following application examples is used is 9950 grades of antimony oxides of technical grade, the ethylene glycol used
For industry terylene level product, the activated carbon used is technical grade powdery, and its size is 100～200 mesh.The analysis of antimony glycol
Method uses the test method in " YS/T972-2014 ethylene glycol antimony powder " standard to test.
Application examples 1
Should the microwave reaction of the use-case method of preparing antimony glycol, comprise the following steps:
0.5L with microwave heating equipment, condensation reflux unit, agitator microwave reaction kettle in, by ethylene glycol and three
Aoxidize two antimony liquid-solid ratioes 2:1, be separately added into ethylene glycol 300mL and antimony oxide 150g, start microwave heating equipment, Microwave Frequency
Rate is 2450MHz, and controlling mixing speed is 30 revs/min, controls reaction temperature 140-145 DEG C, controls condensation reflux unit and goes out
Temperature 90-100 DEG C of gas；When in retort, mixture reaches to control after temperature, during insulation reaction 15 minutes, now, instead
Answer material limpid transparent, add activated carbon 1.2g, then insulated and stirred 10 minutes, be filtrated to get limpid filtrate；Filtrate enters crystallization
Tank, is carried out crystallizing by prior art, the vacuum drying of solid-liquid separation, wet ethylene glycol antimony obtains antimony glycol product 209.5g, its matter
Figureofmerit is: whiteness 93.1%, Sb57.48%, As0.001%, Pb0.0005%, Cu0.0004%, Fe0.0003%；Mother solution microwave
Distillating still distills, and vapo(u)rizing temperature is 120 DEG C～145 DEG C, obtains ethylene glycol, returns and uses；During microwave reaction, second two
Alcohol antimony conversion ratio is 99.45%, the direct yield 96.45% of whole process antimony.
Application examples 2
10L with microwave heating equipment, condensation reflux unit, agitator microwave reaction kettle in, by ethylene glycol and three
Aoxidize two antimony liquid-solid ratioes 3:1, be separately added into ethylene glycol 7500mL and antimony oxide 2500g, start microwave heating equipment, microwave
Frequency is 2450MHz, and controlling mixing speed is 50 revs/min, controls reaction temperature 155-160 DEG C, controls condensation reflux unit
Temperature 100-110 DEG C of exit gas；When in retort, mixture reaches to control after temperature, during insulation reaction 25 minutes, now,
Reaction mass is limpid transparent, adds activated carbon 12.5g, then insulated and stirred 10 minutes, is filtrated to get limpid filtrate；Filtrate enters knot
Brilliant tank, is carried out crystallizing by prior art, the vacuum drying of solid-liquid separation, wet ethylene glycol antimony obtains antimony glycol product 3531.0g, its
Quality index is: whiteness 93.6%, Sb56.78%, As0.0015%, Pb0.0006%, Cu0.0004%, Fe0.0004%；Mother solution is used
Microwave distillation still distills, and vapo(u)rizing temperature is 145～165 DEG C, obtains ethylene glycol, returns and uses；During microwave reaction, second
Glycol antimony conversion ratio is 99.48%, the direct yield 96.36% of whole process antimony.
Application examples 3
10L with microwave heating equipment, condensation reflux unit, agitator microwave reaction kettle in, by ethylene glycol and three
Aoxidize two antimony liquid-solid ratioes 4:1, be separately added into ethylene glycol 7200mL and antimony oxide 1800g, start microwave heating equipment, microwave
Frequency is 2450MHz；Controlling mixing speed is 70 revs/min, controls reaction temperature 170-175 DEG C, controls condensation reflux unit
Temperature 110-120 DEG C of exit gas；When in retort, mixture reaches to control after temperature, during insulation reaction 40 minutes, now,
Reaction mass is limpid transparent, adds activated carbon 12.6g, then insulated and stirred 10 minutes, is filtrated to get limpid filtrate；Filtrate enters knot
Brilliant tank, is carried out crystallizing by prior art, the vacuum drying of solid-liquid separation, wet ethylene glycol antimony obtains antimony glycol product 2514.8g, its
Quality index is: whiteness 93.7%, Sb57.12%, As0.0013%, Pb0.0007%, Cu0.0004%, Fe0.0004%；Mother solution is used
Microwave distillation still distills, and vapo(u)rizing temperature is 165～175 DEG C, obtains ethylene glycol, returns and uses；During microwave reaction, second
Glycol antimony conversion ratio is 99.51%, the direct yield 95.89% of whole process antimony.
Application examples 4
50L with microwave heating equipment, condensation reflux unit, agitator microwave reaction kettle in, by ethylene glycol and three
Aoxidize two antimony liquid-solid ratioes 6:1, be separately added into ethylene glycol 36000mL and antimony oxide 6000g, start microwave heating equipment, micro-
Wave frequency is 915MHz；Controlling mixing speed is 90 revs/min, controls reaction temperature 180-185 DEG C, controls condensation reflux unit
Temperature 110-120 DEG C of exit gas；When in retort, mixture reaches to control after temperature, during insulation reaction 50 minutes, now,
Reaction mass is limpid transparent, adds activated carbon 66g, then insulated and stirred 10 minutes, is filtrated to get limpid filtrate；Filtrate enters crystallization
Tank, is carried out crystallizing by prior art, the vacuum drying of solid-liquid separation, wet ethylene glycol antimony obtains antimony glycol product 8466.6g, its matter
Figureofmerit is: whiteness 93.9%, Sb56.69%, As0.0014%, Pb0.0009%, Cu0.0004%, Fe0.0003%；Mother solution is with micro-
Ripple distillating still distills, and vapo(u)rizing temperature is 175～185 DEG C, obtains ethylene glycol, returns and uses；During microwave reaction, second two
Alcohol antimony conversion ratio is 99.61%, the direct yield 96.12% of whole process antimony.
Application examples 5
50L with microwave heating equipment, condensation reflux unit, agitator microwave reaction kettle in, by ethylene glycol and three
Aoxidize two antimony liquid-solid ratioes 8:1, be separately added into ethylene glycol 40000mL and antimony oxide 5000g, start microwave heating equipment, micro-
Wave frequency is 915MHz；Controlling mixing speed is 100 revs/min, controls reaction temperature 185-190 DEG C, controls condensing reflux dress
Put temperature 110-120 DEG C of exit gas；When in retort, mixture reaches to control after temperature, during insulation reaction 55 minutes, this
Time, reaction mass is limpid transparent, adds activated carbon 60g, then insulated and stirred 10 minutes, is filtrated to get limpid filtrate；Filtrate enters
Crystallizer, is carried out crystallizing by prior art, the vacuum drying of solid-liquid separation, wet ethylene glycol antimony obtains antimony glycol product 7030.1g,
Its quality index is: whiteness 94.2%, Sb57.09%, As0.0015%, Pb0.0004%, Cu0.0004%, Fe0.0002%；Mother solution
Distilling with microwave distillation still, vapo(u)rizing temperature is 180～190 DEG C, obtains ethylene glycol, returns and uses；During microwave reaction,
Antimony glycol conversion ratio is 99.63%, the direct yield 96.45% of whole process antimony.
Application examples 6
2.0L with microwave heating equipment, condensation reflux unit, agitator microwave reaction kettle in, by ethylene glycol and three
Aoxidize two antimony liquid-solid ratioes 10:1, be separately added into ethylene glycol 1000mL and antimony oxide 100g, start microwave heating equipment, microwave
Frequency is 2450MHz；Controlling mixing speed is 30 revs/min, controls reaction temperature 170-175 DEG C, controls condensation reflux unit
Temperature 90-100 DEG C of exit gas；When in retort, mixture reaches to control after temperature, during insulation reaction 15 minutes, now,
Reaction mass is limpid transparent, adds activated carbon 1.0g, then insulated and stirred 10 minutes, is filtrated to get limpid filtrate；Filtrate enters knot
Brilliant tank, is carried out crystallizing by prior art, the vacuum drying of solid-liquid separation, wet ethylene glycol antimony obtains antimony glycol product 139.7g, its
Quality index is: whiteness 93.1%, Sb57.48%, As0.001%, Pb0.0005%, Cu0.0004%, Fe0.0003%；Mother solution is with micro-
Ripple distillating still distills, and vapo(u)rizing temperature is 185～195 DEG C, obtains ethylene glycol, returns and uses；During microwave reaction, second two
Alcohol antimony conversion ratio is 99.45%, the direct yield 96.45% of whole process antimony.
Application examples 7
Example 5 its chemical composition of reaction mother liquor 1000mL(is: Sb 0.95g/L, As 0.071g/L, Pb
0.0051g/L, Cu 0.0005g/L) be placed in microwave distillation still carry out atmospheric evaporation rectification reclaim ethylene glycol, open microwave (control
Microwave power is 600W), stirring, after 5 minutes, temperature rises to 180～190 DEG C, and a large amount of glycol steam enter in condensing tube, 10
After minute, 1000mL mother solution has all distilled, and reclaims and obtains ethylene glycol 950mL, and its chemical composition is: Sb 0.35g/L, As
0.034g/L、Pb 0.0031g/L、Cu 0.0001g/L。
Comparative example 1
At 10L with in the retort of the Resistant heating of condensation reflux unit, liquid-solid with antimony oxide by ethylene glycol
Ratio 6:1, is separately added into ethylene glycol 7.2L and antimony oxide 1200g, starts Resistant heating device；Controlling mixing speed is 90
Rev/min, control reaction temperature 180-185 DEG C, control temperature 110-120 DEG C of condensation reflux unit exit gas；Work as reaction
In-tank mixing thing reaches to control after temperature, and during insulation reaction 156 minutes, now, reaction mass is limpid transparent, adds activated carbon
12g, then insulated and stirred 10 minutes, be filtrated to get limpid filtrate；Filtrate enters crystallizer, then carries out crystallizing, solid-liquid separation, wet
Antimony glycol vacuum drying obtains antimony glycol product 1655.3g, and its quality index is: whiteness 93.1%, Sb57.05%,
As0.0013%, Pb0.0007%, Cu0.0004%, Fe0.0005%；In course of reaction, antimony glycol conversion ratio is 97.12%, whole
The direct yield 94.56% of individual process antimony.With Resistant heating, will reach reaction completely, the response time prolongs significantly with microwave heating
Long, prove further, microwave reaction, be not only offer thermal source, meanwhile, be greatly accelerated response speed.
Comparative example 2
At 10L with in the retort of the Resistant heating of condensation reflux unit, liquid-solid with antimony oxide by ethylene glycol
Ratio 8:1, is separately added into ethylene glycol 8.0L and antimony oxide 1000g, starts Resistant heating device；Controlling mixing speed is
100 revs/min, control reaction temperature 185-190 DEG C, control temperature 110-120 DEG C of condensation reflux unit exit gas；When instead
Answering in-tank mixing thing to reach to control after temperature, during insulation reaction 138 minutes, now, reaction mass is limpid transparent, adds activated carbon
10g, then insulated and stirred 10 minutes, be filtrated to get limpid filtrate；Filtrate enters crystallizer, then carries out crystallizing, solid-liquid separation, wet
Antimony glycol vacuum drying obtains antimony glycol product 1380g, and its quality index is: whiteness 93.3%, Sb56.78%,
As0.0012%, Pb0.0008%, Cu0.0004%, Fe0.0004%；In course of reaction, antimony glycol conversion ratio is 97.45%, whole
The direct yield 94.15% of individual process antimony.With Resistant heating, will reach reaction completely, the response time prolongs significantly with microwave heating
Long, prove further, microwave reaction, be not only offer thermal source, meanwhile, be greatly accelerated response speed.
Comparative example 3
Taking application examples 5 its chemical composition of reaction mother liquor 1000mL(is: Sb 0.95g/L, As 0.071g/L, Pb
0.0051g/L, Cu 0.0005g/L) it is placed in distilling flask and carries out traditional approach Distillation recovery ethylene glycol.Distilling apparatus is two
Mouth alembic, a mouth dress agitating device, a mouth dress condensate recycling device, heats air-distillation on electric furnace and reclaims ethylene glycol.Electricity
Heating (electrical heating power is 600W) after 10 minutes mother solution come to life, continue heating 10 minutes after, 1000mL mother liquid evaporation
250mL, reclaiming its chemical composition of ethylene glycol 240mL(is: Sb 0.036g/L, As 0.035g/L, Pb 0.0037g/L, Cu
0.0002g/L).Amount is microwave distillation amount the 25% of ethylene glycol is evaporated in this distillation within the identical time.Under normal pressure, microwave fills
Put that distillation efficiency is Conventional espresso device 2～4 times.
Claims (5)
1. a microwave reaction prepares the device of antimony glycol, it is characterised in that include microwave reaction kettle, described microwave reaction kettle
By kettle, microwave heating equipment, agitating device, charge door, condensation reflux unit, cover plate, discharge valve, heat-insulation layer and temperature measuring equipment
Composition, described microwave heating equipment is positioned at outside kettle, and described agitating device is positioned in kettle, and is connected with cover plate, described cover plate
Being positioned on kettle to seal kettle, described charge door is positioned on cover plate, and is furnished with lid, and described discharge valve is positioned at kettle lower end,
Described heat-insulation layer is positioned at below kettle, and described condensation reflux unit is positioned on cover plate, and connects with kettle, is used for discharging reaction raw
The water become, described temperature measuring equipment is arranged on the port of export of condensation reflux unit.
Microwave reaction the most according to claim 1 prepares the device of antimony glycol, it is characterised in that also include microwave distillation
Still, described microwave distillation still is by kettle, microwave heating equipment, agitating device, charge door, condensing unit, cover plate, discharge valve, guarantor
Temperature layer and temperature measuring equipment composition, described microwave heating equipment is positioned at outside kettle, and described agitating device is positioned in kettle, and and cover plate
Being connected, described cover plate is positioned on kettle to seal kettle, and described charge door is positioned on cover plate, and is furnished with lid, described discharge valve
Being positioned at kettle lower end, described heat-insulation layer is positioned at below kettle, and described condensing unit is positioned on cover plate, and connects with kettle, is used for
Reclaiming ethylene glycol, described temperature measuring equipment is arranged on the entrance point of condensing unit.
Microwave reaction the most according to claim 1 and 2 prepares the device of antimony glycol, it is characterised in that described microwave adds
Thermal uses annulus or tetragonal body form to carry out being evenly arranged microwave tube, makes microwave uniformly in kettle outer surface.
Microwave reaction the most according to claim 3 prepares the device of antimony glycol, it is characterised in that described condensing reflux fills
Being set to water condensing tube, water condensing tube is furnished with intake-outlet, and is respectively provided with valve, is used for controlling exit gas temperature.
Microwave reaction the most according to claim 4 prepares the device of antimony glycol, it is characterised in that described agitating device is
Anchor agitator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620362807.4U CN205550257U (en) | 2016-04-27 | 2016-04-27 | Device of microwave response preparation ethylene glycol antimony |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620362807.4U CN205550257U (en) | 2016-04-27 | 2016-04-27 | Device of microwave response preparation ethylene glycol antimony |
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| Publication Number | Publication Date |
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| CN205550257U true CN205550257U (en) | 2016-09-07 |
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| CN201620362807.4U Active CN205550257U (en) | 2016-04-27 | 2016-04-27 | Device of microwave response preparation ethylene glycol antimony |
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| Country | Link |
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| CN (1) | CN205550257U (en) |
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2016
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