CN106986798A - One kind synthesis 2, the technique of 4 '-dihydroxydiphenylsulisomer - Google Patents
One kind synthesis 2, the technique of 4 '-dihydroxydiphenylsulisomer Download PDFInfo
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- CN106986798A CN106986798A CN201710200737.1A CN201710200737A CN106986798A CN 106986798 A CN106986798 A CN 106986798A CN 201710200737 A CN201710200737 A CN 201710200737A CN 106986798 A CN106986798 A CN 106986798A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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Abstract
The invention discloses one kind synthesis 2, the technique of 4 '-dihydroxydiphenylsulisomer, with phenol, the concentrated sulfuric acid, between dichlorotoleune, chlorotoluene, the raw material such as homemade nano-magnetic Y2O3/Fe3O4 catalyst passes through recrystallization, magnetic agitation, infrared processing, ultrasonic oscillation prepares 2,4 '-dihydroxydiphenylsulisomer.
Description
Technical field
The present invention relates to a kind of synthesis 2, and the technique of 4 '-dihydroxydiphenylsulisomer belongs to organic synthesis field.
Background technology
2,4 '-dihydroxydiphenylsulisomer (2,4 '-BPS) is white crystal.It can be used not only as the lubrication of tanning material, intermetallic composite coating
Agent, sterilization antiseptic, are largely used to electrothermal sensitive recording paper developer at present, make it have excellent fast light, oil resistant, resistance to absorption
Property, its color developing is more preferable than conventional 4,4 '-dihydroxydiphenylsulisomer (4,4 '-BPS) performance.But synthetic method is commonly used at present
Operation is more complicated, catalyst some costly, the problems such as raw material sources are inconvenient restricts its application.I invents a kind of new
The synthesis technique of type, simple to operate using homemade nano-magnetic Y2O3/Fe3O4 catalyst, yield purity is high.
The content of the invention
Urged in view of the above-mentioned problems of the prior art, the present invention provides one kind using self-control nano-magnetic Y2O3/Fe3O4
Agent synthesis 2, the technique of 4 '-dihydroxydiphenylsulisomer.
To achieve these goals, the technical solution adopted by the present invention is：One kind is using self-control nano-magnetic Y2O3/
Fe3O4 catalyst synthesis 2, the technique of 4 '-dihydroxydiphenylsulisomer.Comprise the following steps：
Step 1, first by phenol under helium atmosphere 180 DEG C of activation process 5h;
Step 2, the phenol after activation is added in container, then homemade nano-magnetic Y2O3/Fe3O4 catalyst is added
Enter, then dichlorotoleune between mixed solvent, chlorotoluene presses 3:1 adds, and then carries out ultrasonication 3h;
Step 3 then again 98% the concentrated sulfuric acid add, it is per minute 20 drop speed be added dropwise, reflux condenser is connected after completion of dropwise addition
Connect to the container, 6h is reacted at 200 DEG C, while opening magnetic agitation；
After step 4, reaction 2h, then water knockout drum is connected to container, moisture is deviate from reflux dewatering processing；
Dichlorotoleune between mixed solvent after step 5, reaction terminate and then using vacuum distillation, chlorotoluene is steamed, and reclaims circulation
Utilize；
Step 6 and then washed with deionized water, then with 5% sodium hydroxide solution alkali cleaning, reclaim homemade nano-magnetic Y2O3/
Fe3O4 catalyst, obtains crude product；
Step 7 and then ethanol solution is first used, recrystallization is handled at 150 DEG C；
Step 8 and then recrystallized again at 150 DEG C of the mixed solution of methylbenzene and ether, then in 120 DEG C of thermostatic drying chamber
Lower drying, finally gives our product 2,4 '-dihydroxydiphenylsulisomer.
Described homemade nano-magnetic Y2O3/Fe3O4 catalyst preparation process：
Step 1, by 1mol/LFeCl33H2O, mixing first carries out ultrasonication to 1mol/LFeCl35H2O solution in equal volume
2h, then in infrared processing 3h;
Step 2 and then 5% sodium hydroxide solution is added drop-wise to above-mentioned solution, while opening magnetic agitation, 100 DEG C of oil bath heatings
3h, detects solution ph, control is in ph values 11 with PH instrument；
Step 3 and then above-mentioned solution is transferred under microwave reactor under nitrogen atmosphere reacts 3h;
After step 4, microwave treatment terminate, nano magnetic particle is separated using magnetic field, deionized water is then first used, then use
Ethanol solution is rinsed, 110 DEG C of dry 2h under rotary evaporator;
Step 5 then by dried nano magnetic particle in Muffle furnace carbon monoxide and nitrogen mixed gas 1:1,600
DEG C, calcine 6h under 0.5kpa, it is last in obtain nano magnetic particle；
Step 6, by 2mol/L yttria solutions carry out infrared radiation processing 2h, then in ultrasonication 2h;
Step 7 and then the yttria solution that nano magnetic particle is added to modification, nanometer will be tentatively obtained by infusion process
Magnetic
Y2O3/Fe3O4 catalyst；
Step 8 and then 2h is dried at 110 DEG C of thermostatic drying chamber, then the calcination processing in tube furnace：In ammonia and blanket of nitrogen
Enclose lower volume and compare 1:4,650 DEG C, under 0.4kpa.5h is calcined, nano-magnetic Y2O3/Fe3O4 catalyst is finally given.
Beneficial effect:It is of the invention a kind of using self-control nanometer magnetic catalyst synthesis 2, the work of 4 '-dihydroxydiphenylsulisomer
Skill, the technological operation is simple, and raw material is relatively easily obtained, and by adding homemade nanometer magnetic catalyst, is effectively raised
Reaction rate, reduces the generation of side reaction, is handled in building-up process by infrared processing etc., can play work to reactant
Change effect enables reaction to be more smoothed out, and reaction is carried out towards expected direction, is improved the yield of target product.It is mixed
The more thorough of impurity removal can be made by closing calcining under gas.Wherein produce phenol and homemade nanometer magnetic catalyst mass ratio 40:3
Sample.Dichlorotoleune, chlorotoluene between phenol 40g, homemade nanometer magnetic catalyst 3g, the 35g98% concentrated sulfuric acid, 200g（3:1）
Mixed solvent.And produce phenol and homemade nanometer magnetic catalyst mass ratio 48:5 sample.Phenol 48g, homemade nanometer
Dichlorotoleune, chlorotoluene between magnetic catalyst 5g, the 35g98% concentrated sulfuric acid, 200g（3:1）Mixed solvent.Made under both ratios
2 obtained, 4 '-dihydroxydiphenylsulisomer yield purity is best.
Embodiment
Embodiment 1
Preparing nano magnetic Y2O3/Fe3O4 catalyst first, step is as follows：
Step 1, by 1mol/LFeCl33H2O, mixing first carries out ultrasonication to 1mol/LFeCl35H2O solution in equal volume
2h, then in infrared processing 3h;
Step 2 and then 5% sodium hydroxide solution is added drop-wise to above-mentioned solution, while opening magnetic agitation, 100 DEG C of oil bath heatings
3h, detects solution ph, control is in ph values 11 with PH instrument；
Step 3 and then above-mentioned solution is transferred under microwave reactor under nitrogen atmosphere reacts 3h;
After step 4, microwave treatment terminate, nano magnetic particle is separated using magnetic field, deionized water is then first used, then use
Ethanol solution is rinsed, 110 DEG C of dry 2h under rotary evaporator;
Step 5 then by dried nano magnetic particle in Muffle furnace carbon monoxide and nitrogen mixed gas 1:1,600
DEG C, calcine 6h under 0.5kpa, it is last in obtain nano magnetic particle；
Step 6, by 2mol/L yttria solutions carry out infrared radiation processing 2h, then in ultrasonication 2h;
Step 7 and then the yttria solution that nano magnetic particle is added to modification, nanometer will be tentatively obtained by infusion process
Magnetic Y2O3/Fe3O4 catalyst；
Step 8 and then 2h is dried at 110 DEG C of thermostatic drying chamber, then the calcination processing in tube furnace：In ammonia and blanket of nitrogen
Enclose lower volume and compare 1:4,650 DEG C, under 0.4kpa, 5h is calcined, nano-magnetic Y2O3/Fe3O4 catalyst is finally given.
2,4 '-dihydroxydiphenylsulisomer is synthetically prepared：Produce phenol and above-mentioned homemade nanometer magnetic catalyst mass ratio
40:3 sample.Dichlorotoleune, chlorotoluene between phenol 40g, homemade nanometer magnetic catalyst 3g, the 35g98% concentrated sulfuric acid, 200g
（3:1）Mixed solvent.
Step 1, first by 40g phenol under helium atmosphere 180 DEG C of activation process 5h;
Step 2, the phenol after activation is added in container, then the homemade nano-magnetic Y2O3/Fe3O4 catalyst of 3g is added
Enter, then dichlorotoleune between 200g mixed solvents, chlorotoluene presses 3:1 adds, and then carries out ultrasonication 3h;
Step 3 and then the 35g98% concentrated sulfuric acid added again, 20 drop speed per minute is added dropwise, reflux condensation mode after completion of dropwise addition
Device is connected to the container, and 6h is reacted at 200 DEG C, while opening magnetic agitation；
After step 4, reaction 2h, then water knockout drum is connected to container, moisture is deviate from reflux dewatering processing；
Dichlorotoleune between mixed solvent after step 5, reaction terminate and then using vacuum distillation, chlorotoluene is steamed, and reclaims circulation
Utilize；
Step 6 and then washed with deionized water, then with 5% sodium hydroxide solution alkali cleaning, reclaim homemade nano-magnetic Y2O3/
Fe3O4 catalyst, obtains crude product；
Step 7 and then ethanol solution is first used, recrystallization is handled at 150 DEG C；
Step 8 and then recrystallized again at 150 DEG C of the mixed solution of methylbenzene and ether, then in 120 DEG C of thermostatic drying chamber
Lower drying, finally gives our product 2,4 '-dihydroxydiphenylsulisomer.
Embodiment 2 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 48：5 sample.Phenol
48g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 3 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 40：5 sample.Phenol
40g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 4 produces phenol and homemade nanometer magnetic catalyst mass ratio 37：5 sample.Phenol 38g, it is homemade to receive
Rice magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 5 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 34：5 sample.Phenol
34g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 6 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 31：5 sample.Phenol
31g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 7 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 28：5 sample.Phenol
48g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 8 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 25：5 sample.Phenol
25g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 9 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 51：5 sample.Phenol
51g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 10 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 54：5 sample.Phenol
54g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 11 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 57：5 sample.Phenol
57g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 12 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 60：5 sample.Phenol
60g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 13 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 63：5 sample.Phenol
48g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 14 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 66：5 sample.Phenol
66g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 15 produces phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 69：5 sample.Phenol
72g, homemade nanometer magnetic catalyst 5g, other raw material dosages, operating procedure is with embodiment 1.
Reference examples 1 produce phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 48：5 sample.Phenol
48g, homemade nanometer magnetic catalyst 5g, not Pyrogentisinic Acid carry out activation process, other raw material dosages, operating procedure is with embodiment
As 1.
Reference examples 2 produce phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 48：5 sample.Phenol
48g, homemade nanometer magnetic catalyst 5g, dichlorotoleune is not that a dichlorotoleune is mixed with chlorotoluene between adding single solvent
Solvent, other raw material dosages, operating procedure is with embodiment 1.
Reference examples 3 produce phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 48：5 sample.Phenol
48g, homemade nanometer magnetic catalyst 5g, it is not that a dichlorotoleune mixes molten with chlorotoluene to add single solvent chlorotoluene
Agent, other raw material dosages, operating procedure is with embodiment 1.
Reference examples 4 produce phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 48：5 sample.Phenol
48g, homemade nanometer magnetic catalyst 5g, without ultrasonication, other raw material dosages, operating procedure is with embodiment 1 one
Sample.
Reference examples 5 produce phenol and homemade nano-magnetic Y2O3/Fe3O4 catalyst qualities ratio 48：5 sample.Phenol
48g, homemade nanometer magnetic catalyst 5g, without magnetic agitation, other raw material dosages, operating procedure is with embodiment 1.
Reference examples 6 produce the sample for being added without homemade nano-magnetic Y2O3/Fe3O4 catalyst, phenol 48g, other raw materials
Consumption, operating procedure is with embodiment 1.
Reference examples 7, which are produced, adds custom catalystses neopelex, other raw material dosages, and operating procedure is with implementing
As example 1.
In order to verify the effect of self-control catalyst, applicant prepares comparative example, and contrast is referred to,
Reference examples 8, in the same manner as in Example 1, difference is that the catalyst applied is different to preparation method, its catalyst preparation
In step 8, the calcination processing in tube furnace：Compare 1 in ammonia and nitrogen atmosphere lower volume:1,650 DEG C, under 0.4kpa, 5h is calcined,
Finally give nano-magnetic Y2O3/Fe3O4 catalyst.
Reference examples 9, in the same manner as in Example 1, difference is that the catalyst applied is different to preparation method, its catalyst system
In standby step 8, the calcination processing in tube furnace：Compare 1 in ammonia and nitrogen atmosphere lower volume:2.
Reference examples 10, in the same manner as in Example 1, difference is that the catalyst applied is different to preparation method, its catalyst
In the step 8 of preparation, the calcination processing in tube furnace：Under single nitrogen atmosphere.
The yield purity of experiment test product：
Liquid chromatogram：ShimadzuLC-10AHPLC;Analytical instrument:Shim-PackVP-ODS posts, Υ 4.6mm × 150mm, post
40 DEG C of temperature, Detection wavelength 254nm, mobile phase:V acetonitriles: V water: V1% phosphoric acid=30: 70: 1, flow 1mL/min, sample is dissolved in second
In nitrile.Detect product component, calculated yield.
Each product 2 of table one, the purity of 4 '-dihydroxydiphenylsulisomer, yield result,
Test result indicates that：It can be found that the technique of embodiment 1,2 obtain 2,4 '-dihydroxydiphenylsulisomer product purity, yield is most
It is good, illustrate proportioning of both techniques in raw material, the production of the operation of technique most beneficial for target product.It is made under other techniques
Product be not especially desirable in purity, yield.Comparative example 2, comparative example 1,2,3,4,5,6,7 is can be found that.No
It is not that a dichlorotoleune is mixed with chlorotoluene that Pyrogentisinic Acid, which carries out dichlorotoleune or chlorotoluene between activation process, the single solvent of addition,
Bonding solvent, without ultrasonication, without magnetic agitation, is added without homemade nanometer magnetic catalyst, adds conventional urge
2 made from agent neopelex, 4 '-dihydroxydiphenylsulisomer purity, yield is not high.Comparative example 8,9,10 can be with
It was found that, make the process conditions of catalyst by oneself（Calcination processing in tube furnace）For product purity, yield has very big influence, in pipe
Calcination processing in formula stove：Compare 1 in ammonia and nitrogen atmosphere lower volume:Under 4 parameters, 2 prepared, the production of 4 '-dihydroxydiphenylsulisomer
Product purity, yield is best, it is seen that the nanometer magnetic catalyst prepared under process conditions, can effectively raise reaction speed
Rate, reduces the generation of side reaction.
Claims (6)
1. one kind synthesis 2, the technique of 4 '-dihydroxydiphenylsulisomer, it is characterised in that:
Step 1, phenol activation is handled first;
Step 2, the phenol after activation is added in container, then homemade nano-magnetic Y2O3/Fe3O4 catalyst is added
Enter, then dichlorotoleune between mixed solvent and chlorotoluene mixing are added, then carry out ultrasonication;
Step 3 then again 98% the concentrated sulfuric acid add, after completion of dropwise addition reflux condenser connection to the container, simultaneously open
Magnetic agitation；
After step 4, reaction, then water knockout drum is connected to container, moisture is deviate from reflux dewatering processing；
Dichlorotoleune between mixed solvent after step 5, reaction terminate and then using vacuum distillation, chlorotoluene is steamed, and reclaims circulation
Utilize；
Step 6 and then washed with deionized water, then with 5% sodium hydroxide solution alkali cleaning, reclaim homemade nano-magnetic Y2O3/
Fe3O4 catalyst, obtains crude product；
Step 7 and then ethanol solution is first used, recrystallization is handled at 150 DEG C；
Step 8 and then recrystallized again at 150 DEG C of the mixed solution of methylbenzene and ether, then in 120 DEG C of thermostatic drying chamber
Lower drying, finally gives 2,4 '-dihydroxydiphenylsulisomer.
2. a kind of synthesis 2 according to claim 1, the technique of 4 '-dihydroxydiphenylsulisomer, it is characterised in that described two
Chlorotoluene and chlorotoluene mass ratio are 3:1.
3. a kind of synthesis 2 according to claim 1, the technique of 4 '-dihydroxydiphenylsulisomer, it is characterised in that described step
Rapid 1 activation process is specially：Phenol 180 DEG C of activation process under helium atmosphere.
4. a kind of synthesis 2 according to claim 1, the technique of 4 '-dihydroxydiphenylsulisomer, it is characterised in that it is described from
The nano-magnetic Y2O3/Fe3O4 method for preparing catalyst of system is as follows：
Step 1, by 1mol/LFeCl33H2O, mixing is first carried out at ultrasonic wave 1mol/LFeCl35H2O solution in equal volume
Reason, then in infrared processing 3h;
Step 2 and then 5% sodium hydroxide solution is added drop-wise to above-mentioned solution, while opening magnetic agitation, 100 DEG C of oil baths add
Heat, detects solution ph, control is in ph values 11 with PH instrument；
Step 3 then by above-mentioned solution be transferred under microwave reactor under nitrogen atmosphere react;
After step 4, microwave treatment terminate, nano magnetic particle is separated using magnetic field, deionized water is then first used, then use
Ethanol solution is rinsed, 110 DEG C of dry 2h under rotary evaporator;
Step 5 then by dried nano magnetic particle in Muffle furnace 600 DEG C of carbon monoxide and nitrogen mixed gas,
Calcine 6h under 0.5kpa, it is last in obtain nano magnetic particle；
Step 6, by 2mol/L yttria solutions carry out infrared radiation processing 2h, then in ultrasonication 2h;
Step 7 and then the yttria solution that nano magnetic particle is added to modification, nanometer will be tentatively obtained by infusion process
Magnetic
Y2O3/Fe3O4 catalyst；
Step 8 and then 2h is dried at 110 DEG C of thermostatic drying chamber, then the calcination processing in tube furnace：In ammonia and blanket of nitrogen
Under enclosing, 650 DEG C, under 0.4kpa, 5h is calcined, nano-magnetic Y2O3/Fe3O4 catalyst is finally given.
5. a kind of synthesis 2 according to claim 4, the technique of 4 '-dihydroxydiphenylsulisomer, it is characterised in that described
Homemade nano-magnetic Y2O3/Fe3O4 method for preparing catalyst in, carbon monoxide and nitrogen mixed gas volume ratio are 1:1.
6. a kind of synthesis 2 according to claim 4, the technique of 4 '-dihydroxydiphenylsulisomer, it is characterised in that the ammonia
Compare 1 with nitrogen atmosphere lower volume:4.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0627415A1 (en) * | 1993-05-31 | 1994-12-07 | Nicca Chemical Co., Ltd. | A method of producing a 2,4'-dihydroxydiphenylsulfone |
| CN101696179A (en) * | 2009-10-27 | 2010-04-21 | 沈阳工业大学 | Method for synthesizing and refining 2,4'-dihydroxy diphenyl sulfone |
-
2017
- 2017-03-30 CN CN201710200737.1A patent/CN106986798A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0627415A1 (en) * | 1993-05-31 | 1994-12-07 | Nicca Chemical Co., Ltd. | A method of producing a 2,4'-dihydroxydiphenylsulfone |
| CN101696179A (en) * | 2009-10-27 | 2010-04-21 | 沈阳工业大学 | Method for synthesizing and refining 2,4'-dihydroxy diphenyl sulfone |
Non-Patent Citations (3)
| Title |
|---|
| 邱明艳，等: "2 [ ( 4 羟基苯基)砜基]苯酚的合成及其精制新工艺", 《应用化学》 * |
| 邱明艳，等: "2[ ( 4羟基苯基)砜基]苯酚的合成及其精制新工艺", 《应用化学》 * |
| 邱明艳，等: "高含量2,4"-二羟基二苯砜的合成", 《化学试剂》 * |
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Application publication date: 20170728 |