CN115650823B - Method for purifying ethylene glycol - Google Patents
Method for purifying ethylene glycol Download PDFInfo
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- CN115650823B CN115650823B CN202211091011.6A CN202211091011A CN115650823B CN 115650823 B CN115650823 B CN 115650823B CN 202211091011 A CN202211091011 A CN 202211091011A CN 115650823 B CN115650823 B CN 115650823B
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- ethylene glycol
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 title claims abstract description 488
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000013078 crystal Substances 0.000 claims abstract description 70
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 238000001816 cooling Methods 0.000 claims abstract description 24
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 238000002425 crystallisation Methods 0.000 claims description 38
- 230000008025 crystallization Effects 0.000 claims description 37
- 238000003756 stirring Methods 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 13
- 235000011089 carbon dioxide Nutrition 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000000746 purification Methods 0.000 abstract description 19
- 239000012535 impurity Substances 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 10
- 238000004781 supercooling Methods 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 8
- 230000006911 nucleation Effects 0.000 abstract description 4
- 238000010899 nucleation Methods 0.000 abstract description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 13
- 239000003245 coal Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 150000002148 esters Chemical class 0.000 description 4
- 238000007710 freezing Methods 0.000 description 4
- 230000008014 freezing Effects 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 210000001787 dendrite Anatomy 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000013094 purity test Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for purifying ethylene glycol, which comprises the following steps: cooling the ethylene glycol sample to a preset temperature; adding an inert crystallizing agent into the ethylene glycol sample to locally generate ethylene glycol seed crystals in the ethylene glycol sample; and solid-liquid separation to obtain pure ethylene glycol. The crystal nucleation rate produced by the purification method is easy to control, the impurity embedding degree is reduced, the purification effect is obviously improved, and meanwhile, the energy consumption is obviously reduced because integral supercooling is not needed. The ethylene glycol obtained by the purification method has high purity and good impurity removal effect.
Description
Technical Field
The invention relates to the technical field of design chemistry purification, in particular to a method for purifying ethylene glycol.
Background
The ethylene glycol production process is mainly divided into petroleum route and coal route. The route of producing ethylene glycol from coal has received much attention. The existing industrial device coal glycol preparation process mainly adopts an oxalate hydrogenation method, which can produce impurities such as multi-carbon alcohol, ethers, esters and the like, and the existing industry generally adopts a multi-stage rectification separation route to remove the impurities. However, trace impurities such as aldehyde and ester are continuously generated in the rectification, the product quality is affected, and the trace impurities such as aldehyde and ester are required to be removed by adopting a melting crystallization mode.
The melting point of ethylene glycol is minus 12.9 ℃, but the metastable zone is wider, and ethylene glycol crystals can be precipitated at a temperature far lower than the freezing point, namely, a supercooling mode is generally adopted to crystallize and precipitate ethylene glycol in raw materials (crude ethylene glycol containing impurities such as aldehyde, ester and the like). However, the supercooling treatment needs excessive supercooling quantity on one hand and consumes more energy; on the other hand, the supersaturation degree is larger, so that the nucleation rate of crystals is extremely high, the embedding of impurities is increased, and the purification effect is reduced.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
Disclosure of Invention
The invention aims to provide a method for purifying ethylene glycol, which can obtain high-purity ethylene glycol and remarkably reduce energy consumption in the purifying process.
To achieve the above object, an embodiment of the present invention provides a method for purifying ethylene glycol, comprising the steps of:
cooling the ethylene glycol sample to a preset temperature;
adding an inert crystallizing agent into the ethylene glycol sample to locally generate ethylene glycol seed crystals in the ethylene glycol sample; and
and (5) carrying out solid-liquid separation to obtain a pure ethylene glycol product.
In one or more embodiments of the present invention, the preset temperature is-12.9 to-30 ℃.
In one or more embodiments of the present invention, cooling the ethylene glycol sample to a preset temperature further comprises:
and cooling the ethylene glycol sample to a preset temperature under the stirring state.
In one or more embodiments of the present invention, the step of cooling the ethylene glycol sample to a preset temperature includes:
and cooling the ethylene glycol sample to a preset temperature, and maintaining the temperature for 0.5-3 h.
In one or more embodiments of the present invention, the inert crystallizing agent is at least one of liquid nitrogen and dry ice.
In one or more embodiments of the invention, the inert crystallization agent to ethylene glycol sample volume ratio is 1: 500-20000.
In one or more embodiments of the present invention, the step of adding an inert crystallization agent to the ethylene glycol sample comprises:
an inert crystallization agent was added to the ethylene glycol sample in a uniform dispersion.
In one or more embodiments of the present invention, the step of adding a uniform dispersion of an inert crystallization agent to the ethylene glycol sample comprises:
an inert crystallization agent was added to the ethylene glycol sample and dispersed with stirring.
In one or more embodiments of the present invention, the step of adding an inert crystallization agent to the ethylene glycol sample to locally seed ethylene glycol in the ethylene glycol sample comprises:
an inert crystallization agent is added to the ethylene glycol sample to locally cool the ethylene glycol sample to produce ethylene glycol seeds.
In one or more embodiments of the present invention, the solid-liquid separation step includes:
and (3) stirring the mixture in the ethylene glycol sample added with the inert crystallizing agent for 0.5-10 h at a stirring speed of 1-800 r/min, and then carrying out solid-liquid separation.
Compared with the prior art, according to the method for purifying the ethylene glycol, the inert crystallizing agent is added into the ethylene glycol sample, so that the ethylene glycol seed crystal is rapidly generated locally in the ethylene glycol sample, and the ethylene glycol in the ethylene glycol sample can be crystallized and separated out under the condition of slightly lower crystallization temperature. The purification method can crystallize without integral supercooling, so that the energy consumption of the whole purification method is obviously reduced. In addition, the nucleation rate of the glycol crystals obtained by the purification method can be controlled by the pre-examination temperature, the impurity embedding degree of the glycol crystals is reduced, and the glycol purification effect is obviously improved.
Drawings
FIG. 1 is a flow chart of a method for purifying ethylene glycol according to an embodiment of the present invention;
FIG. 2 is a graph of the metastable zone width of ethylene glycol.
Detailed Description
The following detailed description of embodiments of the invention is, therefore, to be taken in conjunction with the accompanying drawings, and it is to be understood that the scope of the invention is not limited to the specific embodiments.
As shown in FIG. 2, the melting point of the existing ethylene glycol is minus 12.9 ℃, but the metastable zone is wide, and the ethylene glycol crystals can be separated out at a temperature far below the freezing point, so that the melting crystallization operation is carried out.
Therefore, a common method for purifying coal glycol is a cryogenic method. However, the deep cooling method has the defects of high energy consumption and more embedded crystals.
In addition, the traditional seed crystal method in the crystallization method has the defects of troublesome preparation and preservation and poor repeatability because the traditional seed crystal method needs to break a large crystal into crystal slurry for adding every time, and the crystal size morphology also influences the crystallization effect, so that the operation is troublesome.
As shown in fig. 1, the method for purifying ethylene glycol according to the preferred embodiment of the present invention comprises the steps of:
s1, cooling the ethylene glycol sample to a preset temperature.
Specifically, the pre-examination temperature is lower than the freezing point (freezing point under normal pressure) of ethylene glycol. The higher the pre-examination temperature, the lower the energy consumption of the whole purification process, the slower the crystallization speed of the crystals and the higher the purity of the crystals. The lower the pre-examination temperature is, the relatively higher the energy consumption of the whole purification process is, the relatively faster the crystallization speed of the crystal is, the relatively lower the purity of the crystal is, but the purity of the crystal is higher than that obtained by the conventional supercooling crystallization mode. Preferably, the preset temperature is-12.9 to-30 ℃. The purity can be ensured at the temperature, and the energy consumption is relatively low.
In one embodiment, the ethylene glycol sample may be cooled to a predetermined temperature at a cooling rate of 0.1 to 0.3 ℃/min. In other embodiments, the ethylene glycol sample is cooled to a preset temperature at other cooling rates.
Preferably, the ethylene glycol sample can be cooled to a preset temperature in a stirring state, so that the whole ethylene glycol sample can be uniformly cooled.
Preferably, after the ethylene glycol sample is cooled to the preset temperature, the temperature can be maintained for 0.5-3 hours, so that the temperature of the whole ethylene glycol sample is kept consistent, and the subsequent purity of the ethylene glycol crystal is improved.
S2, adding an inert crystallizing agent into the ethylene glycol sample to locally generate ethylene glycol seed crystals in the ethylene glycol sample.
Specifically, an inert crystallization agent is added to the ethylene glycol sample to locally cool the ethylene glycol sample to produce ethylene glycol seed crystals.
In particular, an inert crystallization agent may be added to the ethylene glycol sample in a uniform dispersion. Therefore, a plurality of seed crystals can be generated in the ethylene glycol sample, which is beneficial to improving the crystallization rate of the ethylene glycol.
Preferably, an inert crystallization agent is added to the ethylene glycol sample and dispersed with stirring. Wherein, stirring can lead the inert crystallization agent to be evenly dispersed and added into the ethylene glycol sample. In addition, the seed crystal generated in the ethylene glycol sample can be broken up by stirring to form smaller seed crystals, and the smaller the seed crystal is uniformly dispersed in the ethylene glycol sample, the less the seed crystal is embedded, the lower the impurity content is, and the higher the purity is.
Specifically, the inert crystallizing agent can be at least one of liquid nitrogen and dry ice. The advantages of selecting liquid nitrogen and dry ice as inert crystallization agents are that: the liquid nitrogen and the dry ice can enable the ethylene glycol sample to be cooled locally, and after the liquid nitrogen and the dry ice are cooled, the liquid nitrogen and the dry ice can sublimate or gasify into gas, so that the pollution to the ethylene glycol sample or the ethylene glycol seed crystal is avoided.
Preferably, the volume ratio of inert crystallization agent to ethylene glycol sample is 1: 500-20000.
In step S2, an appropriate amount of inert crystallization agent is added to the ethylene glycol sample at the preset operation temperature, and the inert crystallization agent is gasified or sublimated to absorb heat, so that the ethylene glycol liquid in the ethylene glycol sample contacted with the inert crystallization agent is supercooled, cooled to an unstable region, and a small amount of ethylene glycol crystals are locally generated in the ethylene glycol sample, thereby achieving the purpose of adding seed crystals in the ethylene glycol melt crystallization process.
In addition, since the volume ratio of the inert crystallization agent to the entire ethylene glycol sample is 1:500 to 20000, i.e. the amount of inert crystallization agent is small and is added as dispersed as possible to the whole ethylene glycol sample, so that small amounts of ethylene glycol crystals are locally generated in the ethylene glycol sample. At this time, a small amount of ethylene glycol crystals is actually an extremely thin crystal film, and therefore the porosity of the crystals is small, dendrites formed during the crystal growth are not formed, and the inclusion of impurities is small, which can be regarded as almost pure ethylene glycol crystals. The existing cryogenic method produces crystals which are monolithic, and the large porosity of the crystals can lead to a large amount of embedding, so that more impurities can be embedded in the glycol crystals.
S3, solid-liquid separation is carried out to obtain the pure ethylene glycol product.
In one embodiment, after the inert crystallizing agent is added into the ethylene glycol sample, the ethylene glycol sample can be kept still for a period of time, so that the seed crystal in the ethylene glycol sample grows to obtain ethylene glycol crystals.
In another embodiment, the ethylene glycol sample added with the inert crystallization agent can be stirred for 0.5 to 10 hours at a stirring speed of 1 to 800r/min, and then subjected to solid-liquid separation. Stirring can play a role in improving the growth speed of ethylene glycol crystals.
The method for purifying ethylene glycol according to the present invention will be described in detail with reference to specific examples.
A single batch of coal ethylene glycol was taken for the following examples.
Example 1
400ml of coal glycol sample is cooled to-25 ℃ at a cooling rate of 0.2 ℃/min under the stirring condition, 1h is maintained, 0.2ml of liquid nitrogen is added into the coal glycol sample, the ethylene glycol seed crystal is instantaneously generated at the part of the sample contacting with the liquid nitrogen, and after the ethylene glycol seed crystal is generated, the stirring speed of 800r/min is carried out, and the stirring is carried out for 0.5 h. And then carrying out solid-liquid separation to obtain ethylene glycol crystals.
Example 2
400ml of a coal-derived ethylene glycol sample was maintained at-25℃with stirring at a rate of 0.1℃per minute for 1 hour, and 0.5cm of the sample was added thereto 3 And (3) generating ethylene glycol seed crystal instantaneously when the solution contacts with the dry ice, and stirring for 10 hours at a stirring speed of 1r/min after generating the ethylene glycol seed crystal. And then carrying out solid-liquid separation to obtain ethylene glycol crystals.
Example 3
400ml of coal glycol sample is cooled to-13 ℃ at a cooling rate of 0.3 ℃/min under the condition of stirring, and is maintained for 1h, and then the mixture is cooled toWherein 1cm is added 3 And (3) generating ethylene glycol seed crystal instantaneously on the part of the sample contacted with the dry ice with the size of the dry ice, and stirring for 1h at a stirring speed of 200r/min after generating the ethylene glycol seed crystal. And then carrying out solid-liquid separation to obtain ethylene glycol crystals.
Comparative example 1
Cooling 50ml of pure ethylene glycol sample to-13deg.C at a cooling rate of 0.2 deg.C/min under stirring, maintaining for 1 hr, and adding 1cm 3 And (3) generating ethylene glycol seed crystal instantaneously on the part of the pure sample contacting with the dry ice, wherein the ethylene glycol pure sample can be totally crystallized after the ethylene glycol seed crystal is generated.
Comparative example 2
Cooling 50ml of pure ethylene glycol sample to-13deg.C at a cooling rate of 0.2 deg.C/min under stirring, maintaining for 1 hr, and adding 0.5cm 3 And (3) generating ethylene glycol seed crystal at the moment when the pure sample contacts with the dry ice, and crystallizing the ethylene glycol pure sample after generating the ethylene glycol seed crystal.
Comparative example 3
400ml of the coal glycol sample is cooled at the cooling rate of 0.2 ℃/min until glycol seed crystals are generated in the sample, and then the mixture is stirred for 0.5h at the stirring speed of 800 r/min. And then carrying out solid-liquid separation to obtain ethylene glycol crystals.
The ethylene glycol crystals obtained in examples 1 to 3 and comparative example 3 were subjected to purity test. The results are shown in the following table:
| purity (%) | Kc (effective distribution coefficient) | |
| Example 1 | 99.95 | 0.010 |
| Example 2 | 99.91 | 0.018 |
| Example 3 | 99.94 | 0.012 |
| Comparative example 3 | 97.50 | 0.500 |
From the purity data of the ethylene glycol crystals obtained in examples 1 to 3 and comparative example 3 in the above table, it can be seen that the purification method of the present invention gives a high ethylene glycol content and a good impurity removal effect.
The effective partition coefficient is used for quantifying the separation result, and the smaller the Kc value is, the better the separation effect is, and the higher the purity of the obtained crystal is. From the above table, examples 1 to 3 have a Kc value during crystallization smaller than that of comparative example 3, thereby demonstrating that the purification method of the present invention has a good purification effect and the obtained crystals have higher purity.
Therefore, the method for purifying the ethylene glycol comprises the steps of adding a proper amount of inert additives with low boiling points such as liquid nitrogen, dry ice and the like into the ethylene glycol raw material liquid with preset operation temperature, gasifying or sublimating the additives to absorb heat, partially supercooling a small amount of raw material liquid contacted with the liquid nitrogen, cooling to an unstable region, and partially generating a small amount of ethylene glycol crystals, thereby achieving the purpose of adding seed crystals in the ethylene glycol melt crystallization process. At this time, the porosity of the crystal is small, dendrites formed during the crystal growth are not formed, and the inclusion of impurities is small, which can be regarded as almost pure glycol crystals. Compared with the whole supercooling operation, the raw material liquid can be crystallized after being cooled to the operation temperature without the whole supercooling operation.
In summary, the method for purifying ethylene glycol of the invention has the following beneficial effects:
1. the crystal nucleation rate produced by the purification method is easy to control, the impurity embedding degree is reduced, the purification effect is obviously improved, and meanwhile, the energy consumption is obviously reduced because integral supercooling is not needed.
2. The glycol obtained by the purification method has high purity and good impurity removal effect.
3. The purification method of the invention is convenient to manufacture and has good repeatability.
4. The purification method of the invention does not need to utilize high-purity liquid to prepare seed crystals by deep cooling in advance and does not need refrigeration storage equipment.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (8)
1. A process for purifying ethylene glycol comprising the steps of:
cooling the ethylene glycol sample to a preset temperature, wherein the preset temperature is-12.9 to-30 ℃;
adding an inert crystallizing agent into the ethylene glycol sample to locally generate ethylene glycol seed crystals in the ethylene glycol sample, wherein the inert crystallizing agent is at least one of liquid nitrogen and dry ice; and
and (5) carrying out solid-liquid separation to obtain a pure ethylene glycol product.
2. The method for purifying ethylene glycol of claim 1, wherein cooling the ethylene glycol sample to a predetermined temperature further comprises:
and cooling the ethylene glycol sample to a preset temperature under the stirring state.
3. The method for purifying ethylene glycol according to claim 1, wherein the step of cooling the ethylene glycol sample to a predetermined temperature comprises:
and cooling the ethylene glycol sample to a preset temperature, and maintaining the temperature for 0.5-3 h.
4. The method for purifying ethylene glycol according to claim 1, wherein the volume ratio of the inert crystallization agent to the ethylene glycol sample is 1: 500-20000.
5. The method for purifying ethylene glycol of claim 1, wherein the step of adding an inert crystallization agent to the ethylene glycol sample comprises:
an inert crystallization agent was added to the ethylene glycol sample in a uniform dispersion.
6. The method for purifying ethylene glycol according to claim 5, wherein the step of adding the inert crystallization agent to the ethylene glycol sample in a uniform dispersion comprises:
an inert crystallization agent was added to the ethylene glycol sample and dispersed with stirring.
7. The method of purifying ethylene glycol of claim 1, wherein the step of adding an inert crystallization agent to the ethylene glycol sample to locally seed ethylene glycol in the ethylene glycol sample comprises:
an inert crystallization agent is added to the ethylene glycol sample to locally cool the ethylene glycol sample to produce ethylene glycol seeds.
8. The method for purifying ethylene glycol according to claim 1, wherein the step of solid-liquid separation comprises:
and (3) stirring the mixture in the ethylene glycol sample added with the inert crystallizing agent for 0.5-10 hours at a stirring speed of 1-800 r/min, and then carrying out solid-liquid separation.
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| CN202211091011.6A CN115650823B (en) | 2022-09-07 | 2022-09-07 | Method for purifying ethylene glycol |
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Citations (5)
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|---|---|---|---|---|
| CN102100975A (en) * | 2011-01-21 | 2011-06-22 | 上海交通大学 | Device and method for purifying ethanediol based on suspension melt crystallization of revolving bed |
| CN103896903A (en) * | 2012-12-26 | 2014-07-02 | 北京奥得赛化学股份有限公司 | Method for preparing and purifying 2,3-O-isopropylidene threitol |
| CN106866371A (en) * | 2015-12-11 | 2017-06-20 | 上海沃凯生物技术有限公司 | A kind of method that utilization fusion-crystallization purifies ethylene glycol |
| CN110759813A (en) * | 2019-10-23 | 2020-02-07 | 太原理工大学 | Method for purifying coal-to-ethylene glycol based on static melt crystallization device |
| CN114315520A (en) * | 2020-10-09 | 2022-04-12 | 中石化南京化工研究院有限公司 | Method for separating and purifying high-carbon diol through low-temperature crystallization |
-
2022
- 2022-09-07 CN CN202211091011.6A patent/CN115650823B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102100975A (en) * | 2011-01-21 | 2011-06-22 | 上海交通大学 | Device and method for purifying ethanediol based on suspension melt crystallization of revolving bed |
| CN103896903A (en) * | 2012-12-26 | 2014-07-02 | 北京奥得赛化学股份有限公司 | Method for preparing and purifying 2,3-O-isopropylidene threitol |
| CN106866371A (en) * | 2015-12-11 | 2017-06-20 | 上海沃凯生物技术有限公司 | A kind of method that utilization fusion-crystallization purifies ethylene glycol |
| CN110759813A (en) * | 2019-10-23 | 2020-02-07 | 太原理工大学 | Method for purifying coal-to-ethylene glycol based on static melt crystallization device |
| CN114315520A (en) * | 2020-10-09 | 2022-04-12 | 中石化南京化工研究院有限公司 | Method for separating and purifying high-carbon diol through low-temperature crystallization |
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