CN106243067A - A kind of purification process of oxolane - Google Patents
A kind of purification process of oxolane Download PDFInfo
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- CN106243067A CN106243067A CN201610679267.7A CN201610679267A CN106243067A CN 106243067 A CN106243067 A CN 106243067A CN 201610679267 A CN201610679267 A CN 201610679267A CN 106243067 A CN106243067 A CN 106243067A
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- oxolane
- purification process
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/04—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
- C07D307/06—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
- C07D307/08—Preparation of tetrahydrofuran
Abstract
The invention discloses the purification process of a kind of oxolane.This purification process includes: oxolane crude product and reducing agent are reacted to remove described peroxide impurity by (1)；(2) will react through the oxolane crude product of step (1) and highly basic or basic anhydride to remove acid impurities；(3) oxolane crude product is passed through adsorbent with except water；(4) by two effect rectifying columns, two effect rectifying columns, oxolane crude product being included the pressurizing tower that atmospheric tower connects with atmospheric tower, the pressure of atmospheric tower is 0.1～0.11MPa, and the pressure of pressurizing tower is 0.7～0.8 MPa.In the purification process of the present invention, it is firstly added reducing agent and removes peroxide impurity, it is subsequently added into highly basic or basic anhydride to remove acid impurities, then by adsorbent with water outlet, azeotrope water and oxolane being formed finally by two effect rectifying columns can preferably separate, thus improve the purity of product, it is ensured that yield.
Description
Technical field
The present invention relates to the technical field that oxolane purifies, particularly relate to the purification process of a kind of oxolane.
Background technology
Oxolane is a kind of organic compound, and oxolane is heterocycle organic compound.It is strong polar ether
One of class, is used as the solvent of a kind of middle polarity when chemical reaction and extraction.Colourless volatile liquid, has the gas of similar ether
Taste.It is dissolved in most organic solvent such as water, ethanol, ether, acetone, benzene.
In prior art, the conventional treatment method of oxolane is reported more, but the research to its method of purification discloses
The fewest.Chinese patent CN105085448 A discloses a kind of adding salt extraction-azeotropic distillation combined process purified tetrahydrofuran
Method, in the method, first wherein removes acid impurities to pending oxolane, then by the suction equipped with modified activated carbon
Attached dose of post carries out adsorption treatment, and the purity after purification is only 99.2wt%, and additionally its yield is relatively low.
Summary of the invention
In view of this, the present invention provides the purification process of a kind of oxolane, through the refined product that this purification process obtains
Purity is higher and yield.
The purification process of a kind of oxolane, it is characterised in that comprise the following steps:
(1) the oxolane crude product comprising oxolane and peroxide impurity and reducing agent are reacted to remove described peroxidating
Thing impurity；
(2) will be anti-through the oxolane crude product comprising oxolane and acid impurities of step (1) and highly basic or basic anhydride
Should be to remove acid impurities；
(3) adsorbent will be passed through with except water through the oxolane crude product comprising oxolane and water of step (2)；
(4) will be included in order to first rectification by two effect rectifying columns, described two effect rectifying columns through the oxolane crude product of step (3)
Atmospheric tower connects and carries out after first rectification the pressurizing tower of rectification again with described atmospheric tower, and the pressure of described atmospheric tower is 0.1
～0.11MPa, the pressure of described pressurizing tower is 0.7～0.8 MPa.
In above-mentioned purification process, in step (1), the addition of reducing agent can be contained peroxide impurity material amount
1～1.05 times, the most such as 1 times, 1.01 times, 1.02 times, 1.03 times, 1.04 times or 1.05 times.Containing of peroxide impurity
Amount can obtain according to known form measurement, such as, can use the means that observation measurements and quantitative measurement combine.This
In, observation measurements specifically, with 10% newly preparation liquor kalii iodide be added in 10 milliliters of oxolanes vibration, have peroxide in
Yellowish-brown.Quantitative measurement specifically, 6 milliliters of acetic acid+1 gram of potassium iodide of+4 milliliters of chloroforms is added to during 50 milliliters of tetrahydrochysenes bark and mutter, dark place
Placing 5 minutes, be titrated to colourless with 0.1N hypo solution, peroxide percentage rate is: N × V × 0.7/G wherein, N, V
Being equivalent concentration and the volume (milliliter) of sodium thiosulfate respectively, G is that tetrahydrochysene is barked the weight (gram) muttered.
As for being reduced the temperature of agent reduction reaction, can be room temperature, such as 20～40 DEG C.Reaction time can be
1～4h, such as 1h, 1.25h, 2h, 2.5h, 3h, 3.5h, 4h etc..
It will be readily understood by those persons skilled in the art that and through the product mixtures of reducing agent reaction, isolate four from above-mentioned
The mode of hydrogen furan, can use distillation.Specifically, add reducing agent in oxolane crude product, and it is stirred continuously, after aoxidizing
Mixture in distill.Means as distillation can use known form, no longer describes in detail in this.
Reducing agent can list lithium aluminium hydride, calcium hydride, sodium borohydride, ferrous chloride and combination in any thereof etc., is preferably
Lithium aluminium hydride, calcium hydride, sodium borohydride, to avoid the introducing of the moisture content using ferrous chloride to be brought.The present invention is not limited to
This.
In step (2), the mode removing acid impurities is to use the mode of filtration.Specifically, add highly basic or alkalescence
Oxide, is allowed to react, and can generate precipitation of salts thing, stratification after reaction, and upper strata is organic layer, and lower floor is water layer, discards
Water layer, retains organic layer, then filters this organic layer, retains filtrate.
Highly basic can list alkali metal hydroxide or C1～4Alcohol alkali metal salt.Herein, C1～4Alcohol alkali metal salt ratio is if any second
Sodium alkoxide, potassium ethoxide, Feldalat NM etc..Alkali metal hydroxide has sodium hydroxide, potassium hydroxide etc..Basic anhydride can have oxidation
Sodium, potassium oxide etc..The consumption of highly basic or basic anhydride is 8～9 scopes preferably with the pH in reaction system.
In step (3), adsorbent is the filler having and sloughing water.Adsorbent can list molecular sieve, silica gel, work
The instantiations such as property aluminium oxide, activated carbon or ion exchange resin.
Such as, can use there is the molecular sieve of about 1.0～5.0 angstroms of mean pore size.The specific surface area of molecular sieve can
With 100～1500m3/g.Molecular sieve can use molecular sieve based on zeolite, molecular sieve based on silicon oxide, based on aluminium oxide
Molecular sieve, molecular sieve based on silicon oxide one aluminium oxide or molecular sieve based on silicate one aluminium oxide are as molecular sieve.
As for the dehydration device for loading adsorbent, can be to use tower or the form of post.It is preferably the form using post.
By the speed of adsorbent, be seated in as a example by adsorption column by adsorbent, its through-rate be 5～15 column volumes/hour, such as may be used
Think 5 column volumes/hour, 5.2 column volumes/hour, 5.5 column volumes/hour, 6 column volumes/hour, 8 column volumes/hour, 10 posts
Volume/hour, 11 column volumes/hour, 12 column volumes/hour, 13 column volumes/hour, 14 column volumes/hour, 14.5 column volumes/
Hour or 15 column volumes/hour etc..
Here after term " column volume " refers to that column volume refers to gel dress post, from the base plate of post to the body on gel deposition surface
Long-pending.
In step (4), the pressure of atmospheric tower can be 0.1 MPa, 0.101 MPa, 0.103MPa, 0.105MPa,
0.108MPa, 0.109MPa, 0.11MPa, preferably 0.101 MPa etc..The pressure of pressurizing tower can be 0.7 MPa, 0.7
01MPa, 0.705 MPa, 0.71 MPa, 0.72 MPa, 0.7 5MPa, 0.78MPa, 0.79MPa or 0.8MPa, preferably 0.74
MPa etc..
Treat the oxolane crude product of rectification from the bottom feed of atmospheric tower, the top discharge of atmospheric tower is content of tetrahydrofuran
Higher target head fraction.This target head fraction is from its top feed of pressurizing tower, and the discharging from the bottom of pressurizing tower is tetrahydrochysene furan
(the most whole rectification terminates the tetrahydrochysene collected to the target fraction again of content of muttering higher (content of tetrahydrofuran is higher than target head fraction)
Furan).You need to add is that, from the fraction of the bottom discharge of atmospheric tower due to the content very trace of its oxolane, can be straight
Connect and discard this fraction.But, from the fraction (being designated as midbarrel) of the discharging at pressurizing tower top due to containing can not ignore content
Oxolane, thus can continue this fraction to be fed to atmospheric tower to be fed to pressurizing tower again.Atmospheric tower and pressurizing tower
Plate number and height etc. can be identical.
It addition, the sum of series internal diameter of divided wall column the most particularly limits, for example, it is contemplated that to the composition of charging, can be based on
The theoretical cam curve calculated by distillation curve is to design described tower.
The reflux ratio of atmospheric tower can be 1～1.6, such as 1,1.1,1.3,1.4,1.5,1.55,1.6 etc..
The reflux ratio of pressurizing tower can be preferably 2.8～4, such as 2.8,2.9,3.0,3.4,3.5,3.8,3.9 or 4
Deng.
Terms above " reflux ratio " refers in distillation operation, by rectifying column tower top return backflow flow L in tower with
The ratio of overhead product flow D, i.e. R=L/D.Above-mentioned reflux ratio can obtain preferable separating effect.
Charging (i.e. treating the oxolane crude product of the rectification) flow of atmospheric tower is advisable with 20～80kg/h, such as 20kg/h,
21kg/h, 22kg/h, 25kg/h, 30kg/h, 40kg/h, 60kg/h, 70kg/h, 75kg/h, 78kg/h, 79kg/h or 80kg/h
Deng.
Charging (the most above-mentioned target head fraction) flow of pressurizing tower can be 60～80kg/h, such as 60kg/h, 61kg/h,
62kg/h, 65kg/h, 70kg/h, 75kg/h, 78kg/h, 79kg/h or 80kg/h etc..
Discharging (the target fraction again) flow of pressurizing tower is 120～150 kg/h, such as 120kg/h, 121kg/h,
125kg/h, 130kg/h, 135kg/h, 140kg/h, 145kg/h, 148kg/h, 149kg/h or 150kg/h etc..
Discharging flow as midbarrel can be 460～500 kg/h, such as 460kg/h, 461kg/h, 465kg/
H, 470kg/h, 480kg/h, 490kg/h, 495kg/h, 496kg/h, 497kg/h, 498kg/h, 499kg/h or 150kg/h etc..
The heating source of above-mentioned atmospheric tower and pressurizing tower can be saturated steam, and cryogen can use the water of room temperature.
As used herein, above-mentioned term:
" one ", " a kind of " and " described " are used interchangeably and refer to one or more.
"and/or" for represent the one or both of illustrated situation all it may happen that, such as, A and/or B includes (A
And B) and (A or B).
It addition, all numerical value that the scope stated by end points herein is comprised in the range of including this (such as, 1 to 10 bag
Include 1.4,1.9,2.33,5.75,9.98 etc.).
It addition, the statement of " at least one " herein include one and above all numbers (such as, at least 2, at least
4, at least 6, at least 8, at least 10, at least 25, at least 50, at least 100 etc.).
In the purification process of the present invention, it is firstly added reducing agent and removes peroxide impurity, be subsequently added into highly basic or alkalescence
Oxide, to remove acid impurities, then by adsorbent with water outlet, makes water and oxolane finally by two effect rectifying columns
The azeotrope formed can preferably separate, and thus improves the purity of product, it is ensured that yield.
Detailed description of the invention
Technical scheme is further illustrated below in conjunction with embodiment.
Embodiment 1
Adding sodium borohydride in the oxolane crude product (purity 98.5%) of technical grade, the addition of sodium borohydride is peroxidating
1 times of thing impurity substances amount, and be stirred continuously, at room temperature backflow 1h, it is allowed to react completely.Redistillation goes out oxolane.
In above-mentioned oxolane, addition sodium hydroxide is to regulate pH to 7, and constantly shake makes acid impurities the most anti-
Should；Stratification, upper strata is organic layer, and lower floor is water layer, discards water layer, retains organic layer, then filters this organic layer,
Retain filtrate.
By above-mentioned filtrate with 5 column volumes/hour by the adsorption column of 4A molecular sieve, to remove moisture.
Finally, by dewatered oxolane by two effect rectifying columns.Particularly as follows: by oxolane with the stream of 20kg/h
Measuring from the bottom feed of atmospheric tower, atmospheric tower, with saturated steam as thermal source, with the water of room temperature as coolant, controls atmospheric tower
Pressure is 0.1Mpa, carries out just rectification.After just rectification, the discharging gathering atmospheric tower top is target head fraction.Again will
This target head fraction is with the flow of 60kg/h from its top feed of pressurizing tower, and atmospheric tower is with saturated steam as thermal source, with room temperature
Water be coolant, the pressure controlling atmospheric tower is 0.7Mpa, gathers the discharging of bottom of pressurizing tower and is first object and evaporates
Point, and by the midbarrel of the top discharge of pressurizing tower again from 460 kg/h from the bottom feed of atmospheric tower so that midbarrel
By pressurizing tower, obtain the second target fraction again.Merge first object fraction again and the second target fraction again, obtain tetrahydrochysene furan
Mutter.It is 95.1% that this example collects the yield of oxolane, and purity is 99.90% after tested.
Embodiment 2
Adding sodium borohydride in the oxolane crude product (purity 99.0%) of technical grade, the addition of sodium borohydride is peroxidating
1.05 times of thing impurity substances amount, and be stirred continuously, at room temperature backflow 4h, it is allowed to react completely.Redistillation goes out tetrahydrochysene furan
Mutter.
In above-mentioned oxolane, addition sodium hydroxide is to regulate pH to 7, and constantly shake makes acid impurities the most anti-
Should；Stratification, upper strata is organic layer, and lower floor is water layer, discards water layer, retains organic layer, then filters this organic layer,
Retain filtrate.
By above-mentioned filtrate with 15 column volumes/hour by the adsorption column of 4A molecular sieve, to remove moisture.
Finally, by dewatered oxolane by two effect rectifying columns.Particularly as follows: by oxolane with the stream of 80kg/h
Measuring from the bottom feed of atmospheric tower, atmospheric tower, with saturated steam as thermal source, with the water of room temperature as coolant, controls atmospheric tower
Pressure is 0.11Mpa, carries out just rectification.After just rectification, the discharging gathering atmospheric tower top is target head fraction.Again will
This target head fraction is with the flow of 80kg/h from its top feed of pressurizing tower, and atmospheric tower is with saturated steam as thermal source, with room temperature
Water be coolant, the pressure controlling atmospheric tower is 0.8Mpa, gathers the discharging of bottom of pressurizing tower and is first object and evaporates
Point, and by the midbarrel of the top discharge of pressurizing tower again from 500 kg/h from the bottom feed of atmospheric tower so that midbarrel
By pressurizing tower, obtain the second target fraction again.Merge first object fraction again and the second target fraction again, obtain tetrahydrochysene furan
Mutter.It is 95.5% that this example collects the yield of oxolane, and purity is 99.92% after tested.
Embodiment 3
Adding sodium borohydride in the oxolane crude product (purity 99.0%) of technical grade, the addition of sodium borohydride is peroxidating
1.05 times of thing impurity substances amount, and be stirred continuously, at room temperature backflow 1h, it is allowed to react completely.Redistillation goes out tetrahydrochysene furan
Mutter.
In above-mentioned oxolane, addition sodium hydroxide is to regulate pH to 7, and constantly shake makes acid impurities the most anti-
Should；Stratification, upper strata is organic layer, and lower floor is water layer, discards water layer, retains organic layer, then filters this organic layer,
Retain filtrate.
By above-mentioned filtrate with 5 column volumes/hour by the adsorption column of 4A molecular sieve, to remove moisture.
Finally, by dewatered oxolane by two effect rectifying columns.Particularly as follows: by oxolane with the stream of 80kg/h
Measuring from the bottom feed of atmospheric tower, atmospheric tower, with saturated steam as thermal source, with the water of room temperature as coolant, controls atmospheric tower
Pressure is 0.11Mpa, carries out just rectification.After just rectification, the discharging gathering atmospheric tower top is target head fraction.Again will
This target head fraction is with the flow of 60kg/h from its top feed of pressurizing tower, and atmospheric tower is with saturated steam as thermal source, with room temperature
Water be coolant, the pressure controlling atmospheric tower is 0.8Mpa, gathers the discharging of bottom of pressurizing tower and is first object and evaporates
Point, and by the midbarrel of the top discharge of pressurizing tower again from 460 kg/h from the bottom feed of atmospheric tower so that midbarrel
By pressurizing tower, obtain the second target fraction again.Merge first object fraction again and the second target fraction again, obtain tetrahydrochysene furan
Mutter.It is 95.8% that this example collects the yield of oxolane, and purity is 99.92% after tested.
Embodiment 4
Adding sodium borohydride in the oxolane crude product (purity 99.5%) of technical grade, the addition of sodium borohydride is peroxidating
1.02 times of thing impurity substances amount, and be stirred continuously, at room temperature backflow 3h, it is allowed to react completely.Redistillation goes out tetrahydrochysene furan
Mutter.
In above-mentioned oxolane, addition sodium hydroxide is to regulate pH to 7, and constantly shake makes acid impurities the most anti-
Should；Stratification, upper strata is organic layer, and lower floor is water layer, discards water layer, retains organic layer, then filters this organic layer,
Retain filtrate.
By above-mentioned filtrate with 10 column volumes/hour by the adsorption column of 4A molecular sieve, to remove moisture.
Finally, by dewatered oxolane by two effect rectifying columns.Particularly as follows: by oxolane with the stream of 50kg/h
Measuring from the bottom feed of atmospheric tower, atmospheric tower, with saturated steam as thermal source, with the water of room temperature as coolant, controls atmospheric tower
Pressure is 0.105Mpa, carries out just rectification.After just rectification, the discharging gathering atmospheric tower top is target head fraction.Again
By this target head fraction with the flow of 70kg/h from its top feed of pressurizing tower, atmospheric tower is with saturated steam as thermal source, with room
The water of temperature is coolant, and the pressure controlling atmospheric tower is 0.75Mpa, and the discharging of the bottom gathering pressurizing tower is first object again
Fraction, and by the midbarrel of the top discharge of pressurizing tower again from 460 kg/h from the bottom feed of atmospheric tower so that centre evaporates
Divide by pressurizing tower, obtain the second target fraction again.Merge first object fraction again and the second target fraction again, obtain tetrahydrochysene furan
Mutter.It is 96.0% that this example collects the yield of oxolane, and purity is 99.95% after tested.
Embodiment 5
Adding sodium borohydride in the oxolane crude product (purity 98.5%) of technical grade, the addition of sodium borohydride is peroxidating
1.03 times of thing impurity substances amount, and be stirred continuously, at room temperature backflow 3h, it is allowed to react completely.Redistillation goes out tetrahydrochysene furan
Mutter.
In above-mentioned oxolane, addition sodium hydroxide is to regulate pH to 7, and constantly shake makes acid impurities the most anti-
Should；Stratification, upper strata is organic layer, and lower floor is water layer, discards water layer, retains organic layer, then filters this organic layer,
Retain filtrate.
By above-mentioned filtrate with 10 column volumes/hour by the adsorption column of 4A molecular sieve, to remove moisture.
Finally, by dewatered oxolane by two effect rectifying columns.Particularly as follows: by oxolane with the stream of 50kg/h
Measuring from the bottom feed of atmospheric tower, atmospheric tower, with saturated steam as thermal source, with the water of room temperature as coolant, controls atmospheric tower
Pressure is 0.101Mpa, carries out just rectification.After just rectification, the discharging gathering atmospheric tower top is target head fraction.Again
By this target head fraction with the flow of 80kg/h from its top feed of pressurizing tower, atmospheric tower is with saturated steam as thermal source, with room
The water of temperature is coolant, and the pressure controlling atmospheric tower is 0.702Mpa, and the discharging of the bottom gathering pressurizing tower is first object
Fraction again, and by the midbarrel of the top discharge of pressurizing tower again from 480 kg/h from the bottom feed of atmospheric tower so that middle
Fraction passes through pressurizing tower, obtains the second target fraction again.Merge first object fraction again and the second target fraction again, obtain tetrahydrochysene
Furan.It is 96.5% that this example collects tetrahydrochysene furan yield, and purity is 99.96% after tested.
Owing to the numerical range of each technological parameter involved in the present invention can not all embody in the above-described embodiments,
As long as but the most envisioned any numerical value fallen in this numerical range above-mentioned of those skilled in the art all can implement this
Invention, the most also includes the combination in any of occurrence in the range of some numerical value.Herein, for the consideration of length, eliminate to
Going out the embodiment of occurrence in certain one or more numerical range, this disclosure being not to be construed as technical scheme is not filled
Point.
Applicant states, the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, i.e. do not mean that the present invention have to rely on above-mentioned in detail
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The equivalence of raw material each to product of the present invention is replaced and the interpolation of auxiliary element, concrete way choice etc., all falls within the present invention's
Within the scope of protection domain and disclosure.
Claims (10)
1. the purification process of an oxolane, it is characterised in that comprise the following steps:
(1) the oxolane crude product comprising oxolane and peroxide impurity and reducing agent are reacted to remove described peroxidating
Thing impurity；
(2) will be anti-through the oxolane crude product comprising oxolane and acid impurities of step (1) and highly basic or basic anhydride
Should be to remove acid impurities；
(3) adsorbent will be passed through with except water through the oxolane crude product comprising oxolane and water of step (2)；
(4) will be included in order to first rectification by two effect rectifying columns, described two effect rectifying columns through the oxolane crude product of step (3)
Atmospheric tower connects and carries out after first rectification the pressurizing tower of rectification again with described atmospheric tower, and the pressure of described atmospheric tower is 0.1
～0.11MPa, the pressure of described pressurizing tower is 0.7～0.8 MPa.
Purification process the most according to claim 1, it is characterised in that described reducing agent is lithium aluminium hydride, calcium hydride, boron hydrogen
Change the one in sodium or at least two.
Purification process the most according to claim 1, it is characterised in that described highly basic is alkali metal hydroxide, described alkali
Property oxide is alkali metal oxide.
Purification process the most according to claim 1, it is characterised in that described adsorbent is molecular sieve, silica gel, work
Property aluminium oxide, activated carbon or ion exchange resin.
Purification process the most according to claim 1, it is characterised in that described by the way of adsorbent be, with 5～15 posts
Volume/hour by equipped with the adsorption column of adsorbent.
Purification process the most according to claim 6, it is characterised in that the reflux ratio of described atmospheric tower is 1～1.6.
Purification process the most according to claim 1, it is characterised in that the reflux ratio of described pressurizing tower is 2.8～4.
Purification process the most according to claim 1, it is characterised in that in step (4), the feed rate of described atmospheric tower is
20～80kg/h.
Purification process the most according to claim 1, it is characterised in that the feed rate of described pressurizing tower is 60～80kg/
h。
Purification process the most according to claim 1, it is characterised in that the discharging flow of described pressurizing tower is 120～150
kg/h。
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| CN108191795A (en) * | 2018-01-26 | 2018-06-22 | 上海星可高纯溶剂有限公司 | The method of purification of chromatographic grade tetrahydrofuran |
| CN109824628A (en) * | 2018-12-13 | 2019-05-31 | 天津康科德医药化工有限公司 | A kind of purification process of chromatography pure tetrahydrofuran |
| CN114031729A (en) * | 2021-12-14 | 2022-02-11 | 山西凯迪建材有限公司 | Preparation method of high-efficiency powdery water reducing agent with siloxane structure |
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| CN108191795A (en) * | 2018-01-26 | 2018-06-22 | 上海星可高纯溶剂有限公司 | The method of purification of chromatographic grade tetrahydrofuran |
| CN109824628A (en) * | 2018-12-13 | 2019-05-31 | 天津康科德医药化工有限公司 | A kind of purification process of chromatography pure tetrahydrofuran |
| CN114031729A (en) * | 2021-12-14 | 2022-02-11 | 山西凯迪建材有限公司 | Preparation method of high-efficiency powdery water reducing agent with siloxane structure |
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