CN104774166A - Synthetic method for disulfide diisopropyl xanthate - Google Patents
Synthetic method for disulfide diisopropyl xanthate Download PDFInfo
- Publication number
- CN104774166A CN104774166A CN201510209213.XA CN201510209213A CN104774166A CN 104774166 A CN104774166 A CN 104774166A CN 201510209213 A CN201510209213 A CN 201510209213A CN 104774166 A CN104774166 A CN 104774166A
- Authority
- CN
- China
- Prior art keywords
- xanthate
- weight
- alkali metal
- reaction
- virahol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a synthetic method for disulfide diisopropyl xanthate. The method comprises the following steps that 1, alkali metal alkoxide is synthesized, wherein isopropyl alcohol is used as a starting raw material, tetrahydrofuran is used as reaction solvent, alkali metal hydroxide is added for carrying out a backflow reaction, and then cooling is carried out to obtain an alkali metal alkoxide reaction solution; 2, an xanthate intermediate is synthesized, wherein a water seal pressing method is adopted for slowly dripping carbon disulfide into the alkali metal alkoxide reaction solution to obtain the xanthate intermediate; 3, the xanthate intermediate is activated, wherein water and iodine are added into the xanthate intermediate to carry out an activating reaction to obtain an activated xanthate intermediate; 4, hydrogen peroxide oxidizing is carried out, wherein hydrogen peroxide is slowly dripped into the activated xanthate intermediate to carry out a reaction in a heat-preserving mode to obtain disulfide diisopropyl xanthate mixed liquor; 5, reactive crystallization and purification are carried out, wherein the disulfide diisopropyl xanthate mixed liquor is distilled and cooled to separate out crystals, then water is added, and the disulfide diisopropyl xanthate mixed liquor is stirred and filtered to obtain the high-purity disulfide diisopropyl xanthate. According to the method, the process is simple, the cost is low, and the yield is high.
Description
Technical field
The present invention relates to chemical field, particularly relate to the synthetic method of dithiodiisopropyl xanthate.
Background technology
Compound dithiodiisopropyl xanthate (English name: dithiodiisopropyl xanthate, No. CAS: 105-65-7, molecular formula: C
8h
14o
2s
4, molecular weight: 270.46) be synthetic rubber polymerization molecular weight regulator, the intermediates such as lubricating oil additive, ore floatation agent, sterilant, weedicide; Also can be used as promotor in Rubber processing, natural rubber and latex, styrene-butadiene rubber(SBR) and latex, paracril and reclaimed rubber ultraaccelerator, also can be used for manufacturing adhesive plaster, medical treatment and operation rubber item, rubber overshoes, waterproof cloth, natural rubber cement and latex product etc.
The structural formula of dithiodiisopropyl xanthate is as follows:
At present, the method for the synthesis dithiodiisopropyl xanthate compound reported mainly contains following two kinds:
(1) Good-Rite Nix and Potassium Persulphate are through oxidizing reaction, after filtration, washing, dry preparation.
(2) Good-Rite Nix is after acidifying, by hydrogen peroxide oxidation, through neutralization, filtration, washing, dry preparation.
Above two kinds of methods are all be that starting raw material prepares dithiodiisopropyl xanthate compound with Good-Rite Nix, wherein, the product yield that potassium persulfate oxidation method obtains and purity all lower, suitability for industrialized production can not be met, hydrogen peroxide oxidation method need first through vitriol oil acidifying, carry out hydrogen peroxide oxidation again, also need thereafter to add the acid in soda ash neutralization reaction liquid, Financial cost is higher, technique is loaded down with trivial details, a large amount of saliferous and organic waste water can be produced.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of simple process, cost is low, productive rate is high, the synthetic method of the dithiodiisopropyl xanthate of environmental protection.
For solving the problem, the synthetic method of dithiodiisopropyl xanthate of the present invention, comprises the following steps:
(1) synthetic alkali metal alkoxide:
Be starting raw material with Virahol, add tetrahydrofuran (THF) as reaction solvent, at room temperature add alkali metal hydroxide again, be then warming up to 60 ~ 70 DEG C and carry out back flow reaction, after 0.5 ~ 2h, be cooled to room temperature, obtain reaction of alkali metal alkoxide liquid; The weight of described tetrahydrofuran (THF) is 3 ~ 6 times of described Virahol weight; The weight of described alkali metal hydroxide is 0.5 ~ 0.7 times of described Virahol weight;
(2) synthesize xanthate intermediate:
Adopt water seal platen press, at-5 DEG C ~ 5 DEG C temperature, dithiocarbonic anhydride is slowly dropped in described reaction of alkali metal alkoxide liquid, stir 8 ~ 10h, obtain xanthate intermediate; The weight of described dithiocarbonic anhydride is 1.5 ~ 3 times of described Virahol weight;
(3) xanthate intermediate activated:
In described xanthate intermediate, add the water of described Virahol weight 2 ~ 4 times, then add the iodine of described Virahol weight 0.5 ~ 1.0 times altogether in three batches, at room temperature priming reaction 0.5 ~ 1h, obtains xanthate activated intermediate;
(4) hydrogen peroxide oxidation:
At 50 DEG C ~ 60 DEG C temperature, the hydrogen peroxide of massfraction >=27.5% is slowly dropped in described xanthate activated intermediate, dropwise insulation reaction 3 ~ 5 h, obtain dithiodiisopropyl xanthate mixed solution; The weight of described hydrogen peroxide is 1 ~ 5 times of described Virahol weight;
(5) reactive crystallization purifying:
Described dithiodiisopropyl xanthate mixed solution is warming up to 65 ~ 75 DEG C, air distillation goes out the reaction solvent of described Virahol weight 1 ~ 4 times, Temperature fall is to room temperature, crystallize out, then the water of described Virahol weight 1 ~ 3 times is added, filter after abundant stirring, obtain highly purified dithiodiisopropyl xanthate.
Described step (1) middle alkali metal hydroxide is sodium hydroxide or potassium hydroxide.
Described step (2) in water seal platen press refer to water injected dithiocarbonic anhydride liquid, after stratification, pass into nitrogen pressurization by dithiocarbonic anhydride metered application to described reaction of alkali metal alkoxide liquid.
The present invention compared with prior art has the following advantages:
1, the present invention take Virahol as reaction starting raw material, by forming alkali metal alcoholates with alkali metal hydroxide, react form xanthate intermediate with dithiocarbonic anhydride, and obtain dithiodiisopropyl xanthate through iodo activation, hydrogen peroxide oxidation, reactive crystallization purifying.Whole process adopts continuous synthesis, does not need the purifying of intermediate, directly can prepare dithiodiisopropyl xanthate.
2, the present invention is in synthesis xanthate intermediate Part, distinguishes traditional alkali metal hydroxide addition method in batches, and dithiocarbonic anhydride metered application in reaction of alkali metal alkoxide liquid, is effectively improve the yield of this step reaction by employing water seal platen press.
3, the present invention is before oxidation step, using iodine as activator, xanthate intermediate is activated, thus eliminate xanthate intermediate acidification step not only, improve the yield of oxidation step, shorten the reaction times, and decrease the generation of waste water and the pollution of environment.
4, the present invention is in compounding design, have selected the reaction solvent tetrahydrofuran (THF) and water that are suitable for continuous synthesis, and achieves the direct crystallization purifying of reaction, decrease technological operation step, improve yield and the purity of dithiodiisopropyl xanthate.
5, used in the whole building-up process of the present invention various reaction masses are cheap and easy to get, greatly reduce cost, and processing step are easy, safety, stable reaction, are easy to control, and do not need special conversion unit and the reaction conditions of harshness simultaneously.
6, through carrying out nucleus magnetic resonance, mass spectroscopy and analysis (see Fig. 1, Fig. 2) to synthetic product of the present invention, can determine: synthetic product of the present invention is dithiodiisopropyl xanthate, product purity >=99.0%.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 be synthetic product of the present invention nuclear magnetic resonance data figure (
1h NMR (CDCl
3, 400 MHz, δ, ppm): 1.399-1.415 (d, 12H, J=3.2Hz, 2 × CH3), 5.662 – 5.724 (m, 2H, O-CH) .).
Fig. 2 is the high resolution mass spectrum figure (HRMS (ESI): MH of synthetic product of the present invention
+found 270.9948 (Calcd. mass for C
8h
15o
2s
4=271.4605) .).
Embodiment
embodiment 1the synthetic method of dithiodiisopropyl xanthate, comprises the following steps:
(1) synthetic alkali metal alkoxide:
With Virahol (60.06g, 1.0mol) be starting raw material, (180.18 g) as reaction solvent to add tetrahydrofuran (THF), at room temperature add alkali metal hydroxide (30.03g again, 0.75mol), then be warming up to 65 DEG C and carry out back flow reaction, after 0.5h, be cooled to room temperature, obtain reaction of alkali metal alkoxide liquid.
Wherein: the weight of tetrahydrofuran (THF) is 3 times of Virahol weight; The weight of alkali metal hydroxide is 0.5 times of Virahol weight.
Alkali metal hydroxide is sodium hydroxide.
(2) synthesize xanthate intermediate:
Adopt water seal platen press, at-5 DEG C of temperature, dithiocarbonic anhydride is slowly dropped in reaction of alkali metal alkoxide liquid, stir 8h, obtain xanthate intermediate.
Wherein: the weight of dithiocarbonic anhydride is 1.5 times of Virahol weight.
Water seal platen press refers to injects dithiocarbonic anhydride liquid by water, after stratification, passes into nitrogen pressurization by dithiocarbonic anhydride metered application in reaction of alkali metal alkoxide liquid.
(3) xanthate intermediate activated:
In xanthate intermediate, adding the water of Virahol weight 2 times, (120.12 g), then adds the iodine (30.03g, 0.12mol) of altogether Virahol weight 0.5 times in three batches, and at room temperature priming reaction 0.5h, obtains xanthate activated intermediate.
(4) hydrogen peroxide oxidation:
At 50 DEG C of temperature, the hydrogen peroxide of massfraction >=27.5% is slowly dropped in xanthate activated intermediate, dropwise insulation reaction 3 h, obtain dithiodiisopropyl xanthate mixed solution.
Wherein: the weight of hydrogen peroxide is 2 times of Virahol weight.
(5) reactive crystallization purifying:
Dithiodiisopropyl xanthate mixed solution is warming up to 70 DEG C, air distillation goes out the reaction solvent of Virahol weight 1 times, and (60.06 g), Temperature fall is to room temperature, crystallize out, then (60.06 g) to add the water of Virahol weight 1 times, filter after abundant stirring, obtain the highly purified dithiodiisopropyl xanthate of 192.0 g.
After tested, this dithiodiisopropyl xanthate productive rate is 71%, and purity is 99.5%.
embodiment 2the synthetic method of dithiodiisopropyl xanthate, comprises the following steps:
(1) synthetic alkali metal alkoxide:
With Virahol (60.06g, 1.0mol) be starting raw material, (180.18 g) as reaction solvent to add tetrahydrofuran (THF), at room temperature add alkali metal hydroxide (30.03g again, 0.75mol), then be warming up to 60 DEG C and carry out back flow reaction, after 2h, be cooled to room temperature, obtain reaction of alkali metal alkoxide liquid.
Wherein: the weight of tetrahydrofuran (THF) is 3 times of Virahol weight; The weight of alkali metal hydroxide is 0.5 times of Virahol weight.
Alkali metal hydroxide is sodium hydroxide.
(2) synthesize xanthate intermediate:
Adopt water seal platen press, at 5 DEG C of temperature, dithiocarbonic anhydride is slowly dropped in reaction of alkali metal alkoxide liquid, stir 10h, obtain xanthate intermediate.
Wherein: the weight of dithiocarbonic anhydride is 1.5 times of Virahol weight.
Water seal platen press refers to injects dithiocarbonic anhydride liquid by water, after stratification, passes into nitrogen pressurization by dithiocarbonic anhydride metered application in reaction of alkali metal alkoxide liquid.
(3) xanthate intermediate activated:
In xanthate intermediate, adding the water of Virahol weight 2 times, (120.12 g), then adds the iodine (30.03g, 0.12mol) of altogether Virahol weight 0.5 times in three batches, and at room temperature priming reaction 1h, obtains xanthate activated intermediate.
(4) hydrogen peroxide oxidation:
At 60 DEG C of temperature, the hydrogen peroxide of massfraction >=27.5% is slowly dropped in xanthate activated intermediate, dropwise insulation reaction 5 h, obtain dithiodiisopropyl xanthate mixed solution.
Wherein: the weight of hydrogen peroxide is 2 times of Virahol weight.
(5) reactive crystallization purifying:
Dithiodiisopropyl xanthate mixed solution is warming up to 65 DEG C, air distillation goes out the reaction solvent of Virahol weight 1 times, and (60.06 g), Temperature fall is to room temperature, crystallize out, then (60.06 g) to add the water of Virahol weight 1 times, filter after abundant stirring, obtain the highly purified dithiodiisopropyl xanthate of 202.8 g.
After tested, this dithiodiisopropyl xanthate productive rate is 75%, and purity is 99.6%.
embodiment 3the synthetic method of dithiodiisopropyl xanthate, comprises the following steps:
(1) synthetic alkali metal alkoxide:
With Virahol (60.06g, 1.0mol) for starting raw material, (360.36 g) as reaction solvent to add tetrahydrofuran (THF), at room temperature add alkali metal hydroxide again, then be warming up to 70 DEG C and carry out back flow reaction, after 1h, be cooled to room temperature, obtain reaction of alkali metal alkoxide liquid.
Wherein: the weight of tetrahydrofuran (THF) is 6 times of Virahol weight; The weight of alkali metal hydroxide is 0.6 times of Virahol weight.
Alkali metal hydroxide is sodium hydroxide.
(2) synthesize xanthate intermediate:
Adopt water seal platen press, at 0 DEG C of temperature, dithiocarbonic anhydride is slowly dropped in reaction of alkali metal alkoxide liquid, stir 9h, obtain xanthate intermediate.
Wherein: the weight of dithiocarbonic anhydride is 3 times of Virahol weight.
Water seal platen press refers to injects dithiocarbonic anhydride liquid by water, after stratification, passes into nitrogen pressurization by dithiocarbonic anhydride metered application in reaction of alkali metal alkoxide liquid.
(3) xanthate intermediate activated:
In xanthate intermediate, adding the water of Virahol weight 4 times, (240.24 g), then adds the iodine (60.06g, 0.24mol) of altogether Virahol weight 1.0 times in three batches, and at room temperature priming reaction 0.75h, obtains xanthate activated intermediate.
(4) hydrogen peroxide oxidation:
At 55 DEG C of temperature, the hydrogen peroxide of massfraction >=27.5% is slowly dropped in xanthate activated intermediate, dropwise insulation reaction 4 h, obtain dithiodiisopropyl xanthate mixed solution.
Wherein: the weight of hydrogen peroxide is 5 times of Virahol weight.
(5) reactive crystallization purifying:
Dithiodiisopropyl xanthate mixed solution is warming up to 75 DEG C, air distillation goes out the reaction solvent of Virahol weight 4 times, and (240.24 g), Temperature fall is to room temperature, crystallize out, then (180.18 g) to add the water of Virahol weight 3 times, filter after abundant stirring, obtain the highly purified dithiodiisopropyl xanthate of 197.4 g.
After tested, this dithiodiisopropyl xanthate productive rate is 73%, and purity is 99.4%.
embodiment 4the synthetic method of dithiodiisopropyl xanthate, comprises the following steps:
(1) synthetic alkali metal alkoxide:
With Virahol (60.06g, 1.0mol) for starting raw material, (360.36 g) as reaction solvent to add tetrahydrofuran (THF), at room temperature add alkali metal hydroxide again, then be warming up to 65 DEG C and carry out back flow reaction, after 2h, be cooled to room temperature, obtain reaction of alkali metal alkoxide liquid.
Wherein: the weight of tetrahydrofuran (THF) is 6 times of Virahol weight; The weight of alkali metal hydroxide is 0.7 times of Virahol weight.
Alkali metal hydroxide is sodium hydroxide.
(2) synthesize xanthate intermediate:
Adopt water seal platen press, at-5 DEG C of temperature, dithiocarbonic anhydride is slowly dropped in reaction of alkali metal alkoxide liquid, stir 10h, obtain xanthate intermediate.
Wherein: the weight of dithiocarbonic anhydride is 2 times of Virahol weight.
Water seal platen press refers to injects dithiocarbonic anhydride liquid by water, after stratification, passes into nitrogen pressurization by dithiocarbonic anhydride metered application in reaction of alkali metal alkoxide liquid.
(3) xanthate intermediate activated:
In xanthate intermediate, adding the water of Virahol weight 2 times, (120.12 g), then adds the iodine (60.06g, 0.24mol) of altogether Virahol weight 1.0 times in three batches, and at room temperature priming reaction 1h, obtains xanthate activated intermediate.
(4) hydrogen peroxide oxidation:
At 60 DEG C of temperature, the hydrogen peroxide of massfraction >=27.5% is slowly dropped in xanthate activated intermediate, dropwise insulation reaction 5 h, obtain dithiodiisopropyl xanthate mixed solution.
Wherein: the weight of hydrogen peroxide is 5 times of Virahol weight.
(5) reactive crystallization purifying:
Dithiodiisopropyl xanthate mixed solution is warming up to 70 DEG C, air distillation goes out the reaction solvent of Virahol weight 4 times, and (240.24 g), Temperature fall is to room temperature, crystallize out, then (120.12 g) to add the water of Virahol weight 2 times, filter after abundant stirring, obtain the highly purified dithiodiisopropyl xanthate of 219.0 g.
After tested, this dithiodiisopropyl xanthate productive rate is 81%, and purity is 99.1%.
embodiment 5the synthetic method of dithiodiisopropyl xanthate, comprises the following steps:
(1) synthetic alkali metal alkoxide:
With Virahol (60.06g, 1.0mol) be starting raw material, (360.36 g) as reaction solvent to add tetrahydrofuran (THF), at room temperature add alkali metal hydroxide (40.0g again, 1.0mol), then be warming up to 65 DEG C and carry out back flow reaction, after 2h, be cooled to room temperature, obtain reaction of alkali metal alkoxide liquid.
Wherein: alkali metal hydroxide is potassium hydroxide.
(2) synthesize xanthate intermediate:
Adopt water seal platen press, at-5 DEG C of temperature, dithiocarbonic anhydride (114.21g, 1.5mol) is slowly dropped in reaction of alkali metal alkoxide liquid, stir 10h, obtain xanthate intermediate.
Wherein: water seal platen press refers to injects dithiocarbonic anhydride liquid by water, after stratification, pass into nitrogen pressurization by dithiocarbonic anhydride metered application in reaction of alkali metal alkoxide liquid.
(3) xanthate intermediate activated:
In xanthate intermediate, add the water of Virahol weight 3 times, then add the iodine of Virahol weight 0.8 times altogether in three batches, at room temperature priming reaction 1h, obtains xanthate activated intermediate.
(4) hydrogen peroxide oxidation:
At 60 DEG C of temperature, the hydrogen peroxide of massfraction >=27.5% is slowly dropped in xanthate activated intermediate, dropwise insulation reaction 5 h, obtain dithiodiisopropyl xanthate mixed solution.
Wherein: the weight of hydrogen peroxide is 1 times of Virahol weight.
(5) reactive crystallization purifying:
Dithiodiisopropyl xanthate mixed solution is warming up to 70 DEG C, air distillation goes out the reaction solvent of Virahol weight 3 times, Temperature fall is to room temperature, crystallize out, then (120.12 g) to add the water of Virahol weight 2 times, filter after abundant stirring, obtain the highly purified dithiodiisopropyl xanthate of 224.4 g.
After tested, this dithiodiisopropyl xanthate productive rate is 83%, and purity is 99.0%.
embodiment 6the synthetic method of dithiodiisopropyl xanthate, comprises the following steps:
(1) synthetic alkali metal alkoxide:
With Virahol (60.06g, 1.0mol) be starting raw material, (360.36 g) as reaction solvent to add tetrahydrofuran (THF), at room temperature add alkali metal hydroxide (40.0g again, 1.0mol), then be warming up to 65 DEG C and carry out back flow reaction, after 2h, be cooled to room temperature, obtain reaction of alkali metal alkoxide liquid.
Wherein: alkali metal hydroxide is sodium hydroxide.
(2) synthesize xanthate intermediate:
Adopt water seal platen press, at-5 DEG C of temperature, dithiocarbonic anhydride is slowly dropped in reaction of alkali metal alkoxide liquid, stir 10h, obtain xanthate intermediate.
Wherein: the weight of dithiocarbonic anhydride is 2 times of Virahol weight.
Water seal platen press refers to injects dithiocarbonic anhydride liquid by water, after stratification, passes into nitrogen pressurization by dithiocarbonic anhydride metered application in reaction of alkali metal alkoxide liquid.
(3) xanthate intermediate activated:
In xanthate intermediate, adding the water of Virahol weight 2 times, (120.12 g), then adds the iodine (60.06g, 0.24mol) of altogether Virahol weight 1.0 times in three batches, and at room temperature priming reaction 1h, obtains xanthate activated intermediate.
(4) hydrogen peroxide oxidation:
At 60 DEG C of temperature, the hydrogen peroxide of massfraction >=27.5% is slowly dropped in xanthate activated intermediate, dropwise insulation reaction 5 h, obtain dithiodiisopropyl xanthate mixed solution.
Wherein: the weight of hydrogen peroxide is 4 times of Virahol weight.
(5) reactive crystallization purifying:
Dithiodiisopropyl xanthate mixed solution is warming up to 70 DEG C, air distillation goes out the reaction solvent of Virahol weight 3 times, and (180.18 g), Temperature fall is to room temperature, crystallize out, then (120.12 g) to add the water of Virahol weight 2 times, filter after abundant stirring, obtain the highly purified dithiodiisopropyl xanthate of 210.9 g.
After tested, this dithiodiisopropyl xanthate productive rate is 78%, and purity is 99.3%.
Claims (3)
1. the synthetic method of dithiodiisopropyl xanthate, comprises the following steps:
(1) synthetic alkali metal alkoxide:
Be starting raw material with Virahol, add tetrahydrofuran (THF) as reaction solvent, at room temperature add alkali metal hydroxide again, be then warming up to 60 ~ 70 DEG C and carry out back flow reaction, after 0.5 ~ 2h, be cooled to room temperature, obtain reaction of alkali metal alkoxide liquid; The weight of described tetrahydrofuran (THF) is 3 ~ 6 times of described Virahol weight; The weight of described alkali metal hydroxide is 0.5 ~ 0.7 times of described Virahol weight;
(2) synthesize xanthate intermediate:
Adopt water seal platen press, at-5 DEG C ~ 5 DEG C temperature, dithiocarbonic anhydride is slowly dropped in described reaction of alkali metal alkoxide liquid, stir 8 ~ 10h, obtain xanthate intermediate; The weight of described dithiocarbonic anhydride is 1.5 ~ 3 times of described Virahol weight;
(3) xanthate intermediate activated:
In described xanthate intermediate, add the water of described Virahol weight 2 ~ 4 times, then add the iodine of described Virahol weight 0.5 ~ 1.0 times altogether in three batches, at room temperature priming reaction 0.5 ~ 1h, obtains xanthate activated intermediate;
(4) hydrogen peroxide oxidation:
At 50 DEG C ~ 60 DEG C temperature, the hydrogen peroxide of massfraction >=27.5% is slowly dropped in described xanthate activated intermediate, dropwise insulation reaction 3 ~ 5 h, obtain dithiodiisopropyl xanthate mixed solution; The weight of described hydrogen peroxide is 1 ~ 5 times of described Virahol weight;
(5) reactive crystallization purifying:
Described dithiodiisopropyl xanthate mixed solution is warming up to 65 ~ 75 DEG C, air distillation goes out the reaction solvent of described Virahol weight 1 ~ 4 times, Temperature fall is to room temperature, crystallize out, then the water of described Virahol weight 1 ~ 3 times is added, filter after abundant stirring, obtain highly purified dithiodiisopropyl xanthate.
2. the synthetic method of dithiodiisopropyl xanthate as claimed in claim 1, is characterized in that: described step (1) middle alkali metal hydroxide is sodium hydroxide or potassium hydroxide.
3. the synthetic method of dithiodiisopropyl xanthate as claimed in claim 1, it is characterized in that: described step (2) in water seal platen press refer to water injected dithiocarbonic anhydride liquid, after stratification, pass into nitrogen pressurization by dithiocarbonic anhydride metered application to described reaction of alkali metal alkoxide liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510209213.XA CN104774166A (en) | 2015-04-28 | 2015-04-28 | Synthetic method for disulfide diisopropyl xanthate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510209213.XA CN104774166A (en) | 2015-04-28 | 2015-04-28 | Synthetic method for disulfide diisopropyl xanthate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104774166A true CN104774166A (en) | 2015-07-15 |
Family
ID=53615971
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510209213.XA Pending CN104774166A (en) | 2015-04-28 | 2015-04-28 | Synthetic method for disulfide diisopropyl xanthate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104774166A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384669A (en) * | 2015-12-09 | 2016-03-09 | 中南大学 | Preparation method of xanthate |
| CN106380436A (en) * | 2016-08-10 | 2017-02-08 | 山东阳谷华泰化工股份有限公司 | Preparation method for diisopropyl xanthogen disulfide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3804771A (en) * | 1972-09-13 | 1974-04-16 | Dart Ind Inc | Thermogenic systems |
| CN102690218A (en) * | 2012-04-27 | 2012-09-26 | 中南大学 | Method for synthesizing xanthate |
| CN103130693A (en) * | 2013-03-12 | 2013-06-05 | 兰州精细化工高新技术开发公司 | Method for synthesizing bis-iso-propyl xanthogenat by using hydrogen peroxide |
-
2015
- 2015-04-28 CN CN201510209213.XA patent/CN104774166A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3804771A (en) * | 1972-09-13 | 1974-04-16 | Dart Ind Inc | Thermogenic systems |
| CN102690218A (en) * | 2012-04-27 | 2012-09-26 | 中南大学 | Method for synthesizing xanthate |
| CN103130693A (en) * | 2013-03-12 | 2013-06-05 | 兰州精细化工高新技术开发公司 | Method for synthesizing bis-iso-propyl xanthogenat by using hydrogen peroxide |
Non-Patent Citations (1)
| Title |
|---|
| LATONGLILA JAMIR等: "Efficient one-pot preparation of bisalkyl xanthogen disulfides from alcohols", 《JOURNAL OF SULFUR CHEMISTRY》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384669A (en) * | 2015-12-09 | 2016-03-09 | 中南大学 | Preparation method of xanthate |
| WO2017097156A1 (en) * | 2015-12-09 | 2017-06-15 | 中南大学 | Preparation method of xanthate |
| CN105384669B (en) * | 2015-12-09 | 2018-02-27 | 中南大学 | The preparation method of xanthates |
| CN106380436A (en) * | 2016-08-10 | 2017-02-08 | 山东阳谷华泰化工股份有限公司 | Preparation method for diisopropyl xanthogen disulfide |
| CN106380436B (en) * | 2016-08-10 | 2018-06-01 | 山东阳谷华泰化工股份有限公司 | A kind of preparation method of dithiodiisopropyl xanthate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101891621B (en) | Compounding method for 3- ethyoxyl-4-ethoxycarbonyl phenylacetic acid | |
| CN104610161A (en) | Preparation method for telmisartan | |
| CN105153110A (en) | Synthesis method for chiral intermediate of atorvastatin calcium | |
| CN102180842B (en) | Synthesis method of 2-amino-delta 2-thiazoline-4-carboxylic acid | |
| CN104774166A (en) | Synthetic method for disulfide diisopropyl xanthate | |
| CN102190592A (en) | Synthetic method of methanamide compound | |
| CN105017030A (en) | Preparation method of 2,2'-bistrifluoromethyl-4,4'-diaminobiphenyl | |
| CN101100450A (en) | Method for preparing ethylsulfonyl acetonitrile | |
| CN102827104A (en) | Method for synthesizing rubber vulcanization accelerator CZ by two-step process by using sodium hypochlorite as oxidizer | |
| CN108947758A (en) | A method of catalysis dibenzofurans open loop prepares biphenyl | |
| CN108586399A (en) | A kind of synthetic method of Fei Luokao former times | |
| CN103524305B (en) | Preparation method of 1,3-propanediol derivatives and intermediates | |
| CN108623488B (en) | Synthetic method of aminomethylbenzoic acid | |
| CN106631823A (en) | Preparation method of lorcaserin intermediate | |
| CN102432434B (en) | Method for synthesizing 3-methyl-3-butene-1-ol | |
| CN111004205A (en) | Synthetic method for preparing piperonyl butoxide under catalysis of composite alkali | |
| CN102993131B (en) | Method for preparing cyclohexene oxide by cyclization of o-chlorocyclohexanol | |
| CN106946724A (en) | The synthetic method of the benzyl malonic acid mono ethyl ester of 2 acetylamino of monoamine base inhibitor class intermediate 2 | |
| CN103265616B (en) | N(2)-L-alanyl-L-glutamine synthesis method | |
| CN102285956A (en) | Synthesis process of cyclopentadecanolide | |
| CN102391170B (en) | A kind of preparation method of N, N-diallyl-5-methoxytryptamine hydrochlorides | |
| CN103880811A (en) | Synthetic method of vinyl ethylene carbonate | |
| CN113307729A (en) | Preparation method of high-performance aluminum acetylacetonate | |
| CN102942464B (en) | Synthesis method of compound 1-(2-halogenophenyl)-3-methyl-butanone-1 | |
| CN104059094B (en) | The dimeric synthetic method of 9-borabi cyclo [3.3.1] nonane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150715 |
|
| RJ01 | Rejection of invention patent application after publication |