CN201807204U - Device adopting molecular distillation technology to purify bisphenol A molecule epoxy resin - Google Patents
Device adopting molecular distillation technology to purify bisphenol A molecule epoxy resin Download PDFInfo
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- CN201807204U CN201807204U CN2010202777394U CN201020277739U CN201807204U CN 201807204 U CN201807204 U CN 201807204U CN 2010202777394 U CN2010202777394 U CN 2010202777394U CN 201020277739 U CN201020277739 U CN 201020277739U CN 201807204 U CN201807204 U CN 201807204U
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Abstract
The utility model discloses a device adopting molecular distillation technology to purify bisphenol A molecule epoxy resin, which comprises a film distiller (1) and a molecule distiller (2). The device is characterized in that the upper end of the film distiller (1) is connected with a film section light component tank (11) via a pipeline, the lower end of the film distiller (1) is connected with the molecule distiller (2) via a film section heavy component tank (12), and the molecule distiller (2) is respectively connected with a molecule section light component tank (21) and a molecule section heavy component tank (22). Epoxy equivalent weight of the bisphenol A molecule epoxy resin obtained due to purification ranges from 169 to 176, and the bisphenol A molecule epoxy is high in purity and yield, and is low in cost.
Description
Technical field
The invention belongs to the purification technique field of bisphenol-A molecule epoxy resin, be specifically related to a kind of device that utilizes molecular distillation technique to carry out purifying bisphenol-A molecule epoxy resin.
Background technology
Epoxy resin is a kind of important thermosetting resin kind, be characterized in having the excellent electric insulation performance, characteristic such as resistance to chemical corrosion, good chemical stability and adhesive strength height, can be widely used in chemical industry, light industry, machinery, electrician, water conservancy, traffic, household electrical appliances, automobile, information industry and aerospace industry etc.The most representative kind is bisphenol A diglycidyl ether (DGEBA) in the epoxy resin, and worldwide its output accounts for more than 75% of epoxy resin total output.Its application spreads all over every field, is the basic material of multiple functional epoxy resin, therefore is called as general purpose epoxy resin.The mixture that common commercially available bisphenol A epoxide resin mainly is made up of the different polymerization degree bisphenol A epoxide resin.In epoxy anhydride insulated paint system, owing to there is the hydroxyl that contains in impurity and the polymer bisphenol A epoxide resin, cause the storage stability of epoxy anhydride resin system to reduce, shorten the resin life cycle.In order to improve the storage stability of epoxy anhydride system, prolong the memory time and the service life of system, can adopt bisphenol A with high purity molecule epoxy resin to prepare epoxy anhydride insulated paint system.This just need separate purification to bisphenol A epoxide resin.
Molecular clock is a kind of special liquid-liquid isolation technics, can under XHV, operate, it can make liquid under far below the temperature of its boiling point it be separated according to the difference of molecular motion mean free path, is specially adapted to the separation of higher boiling, thermal sensitivity and readily oxidizable substance system.So-called molecular motion free path be exactly a molecule between adjacent twice molecular collision the distance of process.At a certain temperature, pressure is low more, and the mean free path of gas molecule is big more.When the pressure of evaporating space is very low, and make condensing surface near evaporating surface, vertical range therebetween is during less than the mean free path of gas molecule, from the vapour molecule of evaporating surface vaporization, can be not and other molecular collisions, directly arrive condensing surface and condensation.Because it has the characteristics such as boiling point, low, the heated time weak point of distillation pressure, separation degree height that vapo(u)rizing temperature is lower than material, thereby can reduce the separation costs of high boiler material greatly, protected the characteristics quality of heat-sensitive substance admirably.Molecular distillation equipment, what application was wider at present is centrifugal thin-film formula and rotor scraped film type.
Though molecular distillation technique should have application aspect some fields of modern industry, yet, because molecular distillation equipment belongs to special equipment, difficulty height such as its preparation cost is high, specification requirement are not found bisphenol-A molecule epoxy special-purpose molecular distillation equipment and application thereof at present as yet.The present invention for this reason.
Summary of the invention
The object of the invention is to provide a kind of device that utilizes molecular distillation technique to carry out purifying bisphenol-A molecule epoxy resin, problem such as solved bisphenol-A molecule epoxy resin poor stability in the prior art, be difficult to purify.
In order to solve these problems of the prior art, technical scheme provided by the invention is:
A kind of separator that utilizes molecular distillation technique to carry out purifying bisphenol-A molecule epoxy resin, comprise film distillator and molecular still, it is characterized in that described film distillator upper end is connected with film section light component jar by pipeline, described film distillator lower end connects molecular still by film section heavy ends jar; Described molecular still connects molecule section light component jar and molecule section heavy ends jar respectively.
Preferably, the described film distillator and the molecular still outside all are provided with heat conductive oil inlet and conduction oil outlet, and when separator was worked, conduction oil entered from heat conductive oil inlet, derive from the conduction oil outlet film distillator or molecular still are heated.
Preferably, molecule section control valve is set between described film section heavy ends jar and molecular still, when film section heavy ends jar is accumulated to when a certain amount of, molecule section control valve is opened the film section heavy component and is entered molecular still.
Preferably, described device also comprises vacuum extractor, and described vacuum extractor connects film distillator and molecular still respectively by pipeline.
Preferably, described device also comprises temperature control equipment, and described temperature control equipment connects film distillator and molecular still respectively by pipeline.
When utilizing above-mentioned device to purify, can adopt following steps to carry out:
(I) be that raw material separates the lighter molecules of removing in the commercially available bisphenol A epoxide resin by film distillator with commercially available bisphenol A epoxide resin, obtain the heavy component of thin-film distillation section;
(II) heavy component with the thin-film distillation section is that raw material separates the bisphenol-A molecule epoxy resin of removing after higher boiling polymer bisphenol A epoxide resin obtains the purification of molecule short-path distillation section in molecular still.
Preferably, in the described method epoxide number of the commercially available bisphenol A epoxide resin of step (I) between 0.51～0.54.
Preferably, the condition that film distillator separates in the described method step (I) comprises that commercially available bisphenol A epoxide resin flows into film distillator with the flow velocity of 800-2000ml/min, vacuum remains 10-100Pa in the described film distillator, and temperature remains 150-200 ℃.
Preferably, step in the described method (I) comprises that also commercially available bisphenol A epoxide resin carries out the raw material degassing and handles before flowing into film distillator, and the temperature that the degassing is handled is at 150-200 ℃, vacuum 10-100Pa.
Preferably, the condition of carrying out the processing of molecule short-path distillation in the described method step (II) comprises the flow velocity inflow molecular still of the heavy component of thin-film distillation section with 600-1500ml/min, vacuum remains 10-50Pa in the described molecular still, and temperature remains 180-250 ℃.
Separation equipment of the present invention can be used for bisphenol A epoxide resin and separates, and the epoxide number of the bisphenol-A molecule epoxy resin that purification is produced is between 0.51～0.54.
Technical solution of the present invention adopts the molecular clock method to prepare the method for bisphenol-A molecule epoxy from common commercially available bisphenol A epoxide resin, and comprise two separation phases: in the thin-film distillation stage, its purpose is to remove little molecules such as low boiling raw material, solvent; And the molecule short-path distillation stage, purpose is to separate higher boiling polymer bisphenol A epoxide resin, obtains product bisphenol-A molecule epoxy resin.Certainly preferred, the thin-film distillation stage need be carried out the raw material pre-treatment, i.e. the degassing is handled, and temperature 150-200 ℃, vacuum 10-100pa.
The epoxide number of the commercially available bisphenol A epoxide resin that technical solution of the present invention is used is between 0.51～0.54; Thin-film distillation is during the stage, and commercially available bisphenol A epoxide resin remains 10-100Pa with the flow velocity inflow vacuum of 800-2000ml/min, and temperature remains 150-200 ℃ thin-film distillation section, removes little molecules such as low boiling raw material, solvent.During molecule short-path distillation separation phase, thin-film distillation section heavy component remains 10-50Pa with the flow velocity inflow vacuum of 600-1500ml/min, temperature remains 180-250 ℃ molecule short-path distillation section, remove higher boiling polymer bisphenol A epoxide resin, obtain product bisphenol-A molecule epoxy resin.
The present invention must remove light components impurity and the bisphenol-A epoxy polymer heavy component that contains alcohol hydroxyl group in the common commercially available bisphenol A epoxide resin earlier in order to obtain bisphenol A with high purity molecule epoxy resin.The present invention preferably adopts the method for rotor scraped film type molecular clock, can produce the purity height, the bisphenol-A molecule epoxy resin that cost is low.The preferred rotor scraped film type molecular clock method that adopts comprises following two separation phases: in the thin-film distillation stage, remove little molecules such as low boiling raw material, solvent; The molecule short-path distillation stage, remove higher boiling polymer bisphenol A epoxide resin, obtain product bisphenol-A molecule epoxy resin.Light component of thin-film distillation section and molecule short-path distillation section heavy component can be used for the common epoxy resins insulation lacquer system that contains and use.The molecular clock process does not have discarded object, pollutant emission, non-environmental-pollution.
Two separation phase specific implementation process of the rotor scraped film type molecular clock process that the present invention preferably adopts are as follows with effect: the thin-film distillation stage, commercially available bisphenol A epoxide resin remains 10-100Pa with the flow velocity inflow vacuum of 800-2000ml/min, temperature remains 150-200 ℃ thin-film distillation section, removes little molecules such as low boiling raw material, solvent; The molecule short-path distillation stage, thin-film distillation section heavy component remains 10-50Pa with the flow velocity inflow vacuum of 600-1500ml/min, temperature remains 180-250 ℃ molecule short-path distillation section, removes higher boiling polymer bisphenol A epoxide resin, obtains product bisphenol-A molecule epoxy resin.
With respect to scheme of the prior art, advantage of the present invention is:
Through the separation of purifying of the device of technical solution of the present invention, the epoxide equivalent of the bisphenol-A molecule epoxy resin of acquisition is between 169～176.By the bisphenol-A molecule epoxy purity height that the molecular clock method prepares, yield is big, and cost is low.
In sum, the present invention discloses a kind of device that adopts the molecular clock method to prepare bisphenol-A molecule epoxy resin from common commercially available bisphenol A epoxide resin, by two separation phases: the thin-film distillation stage, commercially available bisphenol A epoxide resin remains 10-100Pa with the flow velocity inflow vacuum of 800-2000ml/min, temperature remains 150-200 ℃ thin-film distillation section, removes little molecules such as low boiling raw material, solvent; The molecule short-path distillation stage, thin-film distillation section heavy component remains 10-50Pa with the flow velocity inflow vacuum of 600-1500ml/min, temperature remains 180-250 ℃ molecule short-path distillation section, removes higher boiling polymer bisphenol A epoxide resin, obtains product bisphenol-A molecule epoxy resin.By the bisphenol-A molecule epoxy purity height that the molecular clock method prepares, yield is big, and cost is low.Light component of film section and molecule section heavy component can be used for the common epoxy resins insulation lacquer system that contains and use.The molecular clock process does not have discarded object, non-pollutant discharge, non-environmental-pollution.
Description of drawings
Below in conjunction with drawings and Examples the present invention is further described:
Fig. 1 is the structure flow charts of the embodiment of the invention 3 bisphenol A epoxide resins with molecular clock purification separation equipment;
Wherein: 1 is film distillator, and 2 is molecular still, and 4 is vacuum extractor; 5 is the sample generator; 11 is film section light component jar; 12 is film section heavy ends jars; 21 is molecule section light component jar; 22 is molecule section heavy ends jars; 31 is heat conductive oil inlet; 32 are the conduction oil outlet; 33 is molecule section control valve; 34 is handpiece Water Chilling Units.
The specific embodiment
Below in conjunction with specific embodiment such scheme is described further.Should be understood that these embodiment are used to the present invention is described and are not limited to limit the scope of the invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
Embodiment molecular clock purification separation equipment
As shown in Figure 1, this utilizes molecular distillation technique to carry out the separator of purifying bisphenol-A molecule epoxy resin, comprise sample generator 5, film distillator 1, molecular still 2, vacuum extractor 4, temperature control equipment, described film distillator 1 upper end is connected with film section light component jar 11 by pipeline, and described film distillator 1 lower end connects molecular still 2 by film section heavy ends jar 12; Described molecular still 2 connects molecule section light component jar 21 and molecule section heavy ends jar 22 respectively.On the pipeline of film section heavy ends jar 12 and molecular still 2 the flow-control peephole can be set and carry out the manual observation changes in flow rate.
Described sample generator 5 comprises two high-order crude product jars (A, B) arranged side by side, and described high-order crude product jar is connected with vacuum extractor by pipeline, and when starting vacuum extractor, epoxy resin can be drawn into high-order crude product jar respectively.Described sample generator 5 is connected with film distillator by inlet valve.Described high-order crude product jar and film distillator can be provided with flowmeter and measure.
Described temperature control equipment connects film distillator 1 and molecular still 2 respectively by pipeline.Described temperature control equipment comprises the hotline heater that the film distillator 1 and molecular still 2 outsides are set and is arranged on handpiece Water Chilling Units 34 on the pipeline, the described film distillator 1 and molecular still 2 outsides all are provided with heat conductive oil inlet 31 and conduction oil outlet 32, when separator is worked, conduction oil enters from heat conductive oil inlet 31, derives from conduction oil outlet 32 film distillator 1 or molecular still 2 are heated.
Described film section heavy ends jar 12 and 2 of molecular stills are provided with molecule section control valve 33, and when film section heavy ends jar 12 is accumulated to when a certain amount of, molecule section control valve 33 is opened the film section heavy component and entered molecular still.Described vacuum extractor 4 connects film distillator 1 and molecular still 2 respectively by pipeline.Described vacuum extractor 4 comprises vavuum pump group P1 and vavuum pump group P2.Present embodiment intermediate pump group P1 is the vacuum unit; Vavuum pump group P2 is a lobe pump.Vavuum pump group P2 is exclusive to vacuumize for the molecular clock stage; And vavuum pump group P1 can vacuumize for film distillator in the molecular clock stage; Can take out also that district's crude product is former to be expected in the crude product jar and, heavy ends jar light in the molecule section of molecular clock vacuumizes processing by negative pressure.
When carrying out the purification of epoxy resin crude product, can carry out according to following technology:
1, the preliminary treatment of raw material and technological preparation:
Stand-by epoxy resin is poured in 20 kilograms of stands, put into 150 ℃ of drying rooms and be incubated 12h at least.Whether each valve in the testing fixture (particularly containing the vacuum line valve) is in correct position, check whether positions such as circuit, pipeline, visor have breakage, and definite device systems is in normal condition.
2, concrete running:
The open system cooling water valve is adjusted cooling water flow to zone of reasonableness.All power-on comprises vacuum, temperature control panel power supply.Start the slide valve pump of P1 pump group, open pipeline valve towards head tank.With high-order crude product jar A of epoxy resin difference suction and B, each jar can be put 90～100 kilograms (4.5 barrels of about 20 kilograms of stands), and be stand-by.
Take out material and finish, vacuum pipe is switched to the thin-film distillation system, open the atmospheric valve of crude product jar A and B, open heating valve slightly, 150 ℃ of control material temperature are closed heating valve, allow it heat up naturally, in kind heat when the material temperature is lower than 150 ℃ in the use.With film conduction oil inlet valve (reversing valve one circle approximately partly); Temperature on the chain of command version is adjusted to 150 ℃, treats again the control panel temperature to be adjusted to 180 ℃ behind the temperature stabilization.
Open the cooling unit:
Open cooling unit power knob on the master control panel; Open cooling unit self power switch then; Secondly open cooling unit power supply soft key, the design temperature upper limit-10 ℃, lowest temperature-16 ℃; Open cooling fluid import and export circulation valve (two), open the cycle button on the cooling unit chain of command version, observe whether cooling fluid is in recurrent state in the container; Liquid to be cooled is opened on the control panel and is cooled off button after continuing normal circulation operation 10-20min; P1 vacuum unit is switched to the thin-film distillation end, open film section and stir; Treat that the film section vacuum reaches 8.0 * 10
1During Pa, open the lobe pump of P2 pump group, reach 8.0 * 10 to film section vacuum
0Pa; Confirm that film section heat conductive oil inlet temperature has been stabilized in 180 ℃, open charging valve on the film section flowmeter, and adjust charging rate, generally can remain on 1L/5min by flowmeter.The thin-film distillation certain hour, about 1.5h; Film heavy ends jar has accumulated the cut of some.
With molecule conduction oil inlet valve (reversing valve one circle approximately partly); Temperature on the chain of command version is adjusted to 150 ℃, treats again the control panel temperature to be adjusted to 200～210 ℃ behind the temperature stabilization.Open molecule short distance section vacuum valve (comprising all corresponding finished product material-storage jars), open P2 vavuum pump group slide valve pump; Treat that the film section vacuum reaches 8.0 * 10
1During Pa, open the lobe pump of P2 pump group, reach 8.0 * 10 to molecule short distance section vacuum
0Pa; Opening molecule short distance section stirs; Open the valve (by two sections continuous lens the flow velocity of material being estimated, extremely an amount of by the flow velocity of valve regulated material simultaneously) that film is connected with the molecule section, also can control below the molecule section vacuum 5Pa.
Use wherein one group light, heavy ends product collection jar, close another group charging valve; When treating to have material to flow in light, the heavy ends jar, scioptics observe to produce whether be in normal condition.When one group of basin is collected product and will be expired, switch to another group, will the P1 pump temporarily can be switched from film section and come slack tank forvacuum earlier before, charging that at this moment can the Temporarily Closed film section behind the handover success, recovers the normal charging of film section.
The light component of molecule section is in time put into clean bucket.Heavy ends quantity is fewer, can change bucket when deposit is full, and vacuum will be supplied when changing barrel, and it is fast that speed is wanted, otherwise can influence product purity and yield.
End of run:
Produce when finishing, close all heating valves; Close film section vacuum valve and P1 pump group, molecule section light component has certain hysteresis, so molecule section vacuum group and stirring just can be closed after will waiting light component stream intact, last closure molecule section stirs and P2 pump group, closes water source and power supply.
Purification operations can be carried out according to following steps:
Certain commercially available bisphenol A epoxide resin, epoxide number 0.522, uncovered placing more than 150 ℃ of baking oven insulation 12h.According to standard operation, check the molecular clock system, fused raw material is added head tank.The thin-film distillation stage flows into vacuum with the flow velocity of 1000 ± 100ml/min and remains 50 ± 5Pa, and temperature remains 175 ± 5 ℃, removes little molecules such as low boiling raw material, solvent; The molecule short-path distillation stage, thin-film distillation section heavy component remains 20 ± 5Pa with the flow velocity inflow vacuum of 900 ± 50ml/min, temperature remains 200 ± 10 ℃ molecule short-path distillation section, removes higher boiling polymer bisphenol A epoxide resin, obtains product bisphenol-A molecule epoxy resin.After testing, the bisphenol-A molecule epoxy resin epoxide equivalent that makes is 171.1.
Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All spirit essence is done according to the present invention equivalent transformation or modification all should be encompassed within protection scope of the present invention.
Claims (5)
1. device that utilizes molecular distillation technique to carry out purifying bisphenol-A molecule epoxy resin, comprise film distillator (1) and molecular still (2), it is characterized in that described film distillator (1) upper end is connected with film section light component jar (11) by pipeline, described film distillator (1) lower end connects molecular still (2) by film section heavy ends jar (12); Described molecular still (2) connects molecule section light component jar (21) and molecule section heavy ends jars (22) respectively.
2. device according to claim 1 is characterized in that described film distillator (1) and molecular still (2) outside all is provided with heat conductive oil inlet (31) and conduction oil outlet (32).
3. device according to claim 1 is characterized in that between described film section heavy ends jar (12) and molecular still (2) molecule section control valve (33) being set.
4. device according to claim 1 is characterized in that described device also comprises vacuum extractor (4), and described vacuum extractor (4) connects film distillator (1) and molecular still (2) respectively by pipeline.
5. device according to claim 1 is characterized in that described device also comprises temperature control equipment, and described temperature control equipment connects film distillator (1) and molecular still (2) respectively by pipeline.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010202777394U CN201807204U (en) | 2010-07-30 | 2010-07-30 | Device adopting molecular distillation technology to purify bisphenol A molecule epoxy resin |
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| CN2010202777394U CN201807204U (en) | 2010-07-30 | 2010-07-30 | Device adopting molecular distillation technology to purify bisphenol A molecule epoxy resin |
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| CN201807204U true CN201807204U (en) | 2011-04-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914193A (en) * | 2010-07-30 | 2010-12-15 | 苏州巨峰电气绝缘系统股份有限公司 | Method for purifying bisphenol-A molecular epoxy resin by using molecular distillation technology and device thereof |
-
2010
- 2010-07-30 CN CN2010202777394U patent/CN201807204U/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914193A (en) * | 2010-07-30 | 2010-12-15 | 苏州巨峰电气绝缘系统股份有限公司 | Method for purifying bisphenol-A molecular epoxy resin by using molecular distillation technology and device thereof |
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Granted publication date: 20110427 |