CN102690218B - Method for synthesizing xanthate - Google Patents
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Abstract
Disclosed is a method for synthesizing xanthate, relating to a synthetic process of a flotation collector of metal mines. The invention provides a method for synthesizing xanthate with high yield and good quality. The xanthate of the invention is prepared by adopting the technical solution that raw materials comprise alcohol, carbon disulfide, and caustic alkali with a molar ratio of 1:3-9:1-1.1, wherein the caustic alkali is sodium hydroxide or potassium hydroxide, and the xanthate which is known as Huangyao is prepared by reacting the raw materials for 0.5-8 hours at a temperature ranged from 10 DEG C to 70 DEG C. The invention further discloses methods for recycling a carbon disulfide solvent. The first method comprises filtering materials from a reactor under the protection of nitrogen, and carrying out reduced pressure distillation on the obtained filter cake to acquire a xanthate product with high purity and a carbon disulfide solvent. A Filter liquor and the recycled carbon disulfide can be cycledly utilized. The second method comprises first carrying out an atmospheric distillation on materials from the reactor at a temperature ranged from 50 DEG C to 90 DEG C to recover most of the carbon disulfide, and then carrying out reduced pressure distillation to recover the rest of the carbon disulfide and acquire a xanthate product with high purity at the same time.
Description
Technical field
The present invention relates to a kind of solvent method synthesis technique of xanthogenate.
Background technology
Xanthogenate ROCSSNa (K), be commonly called as " xanthate ", can form and can dissolve compound with many kinds of metal ions.1815, Cai Si (Zeise) is synthetic xanthogenate first, because it is yellow, therefore be referred to as xanthate.After Keller found that in nineteen twenty-five xanthate can be used as the flotation collector of sulfide mineral, xanthate was widely used in the metal sulfide mountain to reclaim metal sulfide ore.At present, xanthate is the sulfide flotation collector of mineral manufacture field consumption maximum.
At present, the method for synthetic xanthate mainly contains " kneading method " and " solvent method ".Kneading method is that alcohol and dithiocarbonic anhydride are added to kneading machine, then progressively adds powder alkali (sodium hydroxide or potassium hydroxide), generates xanthate 25 ℃～35 ℃ reactions.Because it does not need other auxiliary materials, need not any solvent, generative process is simple, and cost is lower, be at present the solid xanthate the major industry production method (Tian Xishuan, Wang Yongxin. the xanthate production method is inquired into [J]. non-ferrous metal (ore dressing part) 1991 (03): 30-31; The bear firewood. the production practice of xanthate synthesis technique [J]. copper industrial engineering (IE), 2003 (2): 29-31).But the method needs the alkaline system to pulverize sheet alkali or granulated alkali, and powder alkali water absorbability and corrodibility are strong.The method needs the abundant kneading of raw material simultaneously, strictly controls temperature of reaction, and foreign matter content is high, and xanthate product purity and yield are lower, and particularly unreacted sodium hydroxide is stored in wherein, can cause the decomposition of xanthate, thereby affects the quality of xanthate product.
Solvent method is that alcohol, dithiocarbonic anhydride and alkali are reacted in a certain amount of solvent, has reacted rear steaming and has desolventized and obtain the xanthate product.Solvent method does not need the alkaline system, and chemical reaction carries out all the time in liquid phase, the sodium hydroxide added in process or potassium hydroxide are easy to scatter, solvent can be removed reaction heat in time simultaneously, avoided producing because of local superheating the shortcoming that the impurity such as inorganic sulphide and non-xanthate organic sulfide cause poor product quality, thereby the transformation efficiency of alcohol is high, the yield of xanthate and purity are also high.There is at present the solvent of report to mainly contain the (Shi Xianyi such as benzene, toluene, kerosene, ethylene dichloride, raw alcohol, dimethylbenzene, ethylbenzene, gasoline, Qin Xuemei, Deng Zhongyan. the improvement of Synthesis Process of Sodium n-butyl Xanthate [J]. Chemical Engineering Technology and exploitation, 2006,35 (4): 47-48; Hu Zhengji, Wang Shiyue, Wang Qingjiu, Qu Zhiqiang. solvent method is produced isobutyl-potassium xanthate [J]. coloured mining and metallurgy, 1999 (4): 16-18; Konrad Baessler, Georg Polz.Process for the manufacture of alkali xanthates[P] .AU1713170A, 1970-7-3; Tian Xishuan, Wang Yongxin. the xanthate production method is inquired into [J]. non-ferrous metal (ore dressing part) 1991 (03): 30-31; A.M.Ahmed, K.Ibrahim, O.R.Anna, P.F.Jr John.Synthesis, characterization and luminescent propertiesof dinuclear Gold (I) xanthate complexes:X-ray structure of [Au
2(n-Buxanthate)
2] [J] .Inorg Chem 2004,43:3833-3839; Huang Jun. a kind of synthesis technique of sodium n-butyl-xanthate [P] .CN102050769A, 2011-05-11).According to solvent, whether be reaction raw materials, solvent method can be divided into again to non-raw material solvent method and alcohol excess method.Wherein non-raw material solvent method need be introduced the nonreactants such as benzene, toluene, kerosene, ethylene dichloride, dimethylbenzene, ethylbenzene or gasoline in the xanthate preparation process, can dithiocarbonic anhydride or raw alcohol be brought in non-raw material solvent together completely by the part unreacted during desolventizing, while causing lower secondary response, the metering of dithiocarbonic anhydride or raw alcohol can not be accurate, affects xanthate quality product and yield; These non-raw material solvents of while, boiling point is higher, and the solvent recuperation energy consumption is higher.The alcohol excess method can be eliminated the introducing of non-raw material solvent, but in desolventizing, the water generated during xanthate is synthetic also has part to distill out with the solvent raw alcohol, and water and alcohol have certain intermiscibility, and water and pure separation circuit will directly cause the xanthate manufacturing cost to increase; And pure direct circulation will be introduced water when lower secondary response, have a strong impact on xanthate quality product and yield; And pure boiling point is higher, the solvent recuperation energy consumption is higher.Therefore solvent method is rarely used in industrial production.
2007, M.Alijanianzadeh etc. have reported that laboratory prepares the dithiocarbonic anhydride raw material overflow method (M.Alijanianzadeh of xanthate on a small quantity, A.A.Saboury, H.Mansuri-torshizi, K.Haghbeen, A.A.Moosavi-movahedi.The inhibitory effect of some new synthesized xanthates on mushroom tyrosinase activities[J] .Journal of Enzyme Inhibition and Medicinal Chemistry, 2007,22 (2): 239-246.).The proportioning raw materials alcohol that they adopt: dithiocarbonic anhydride: sodium hydroxide=1: 2: 1 (ratio of amount of substance), because the dithiocarbonic anhydride raw material is excessive, while starting to react, be well on, but reaction late phase reaction material becomes dry fully, stir difficulty, for this reason, they add acetone solvent so that stir smoothly.Owing in reaction mixture, containing dithiocarbonic anhydride and solvent acetone, they do not reclaim excessive dithiocarbonic anhydride raw material, and simultaneously, they only reacted 15 minutes after adding acetone solvent, and the reaction that generates xanthate is incomplete, causes xanthate product purity and yield lower.
Summary of the invention
The synthetic method that the purpose of this invention is to provide a kind of xanthogenate, resulting xanthogenate purity is high, and impurity is few, and method feed stock conversion of the present invention is high, and the required energy consumption of follow-up solvent recuperation is low, and more easily realizes the industrialization cyclic production.
Further object of the present invention is, provides a kind of simple and convenient, can, by the efficient recovery of the excessive dithiocarbonic anhydride that produces in above-mentioned synthetic method, separate the method for recycling.
Technical scheme of the present invention is: the dithiocarbonic anhydride of take is reaction raw materials and solvent, the nitrogen of take is the reaction shielding gas, add in reaction raw materials alcohol, caustic alkali a kind of in two kinds, another kind add alcohol, caustic alkali under 0 ℃～40 ℃ whipped states in two kinds is under 10 ℃～70 ℃, to continue reaction in temperature of reaction; After having reacted, from reaction mixture, isolating excessive dithiocarbonic anhydride, obtain xanthogenate; Described alcohol: dithiocarbonic anhydride: the ratio of the amount of substance of caustic alkali is 1: 3～9: 1～1.1; Described alcohol comprises potato spirit, C
2-C
8One or more of fatty alcohol.
Describedly isolate excessive dithiocarbonic anhydride, reaction mixture is filtered under nitrogen protection, the filter cake underpressure distillation, obtain respectively xanthogenate and dithiocarbonic anhydride; Or after first with nitrogen replacement, falling the air in distillation plant, reaction mixture, first 50 ℃～90 ℃ lower air distillations, is reclaimed to dithiocarbonic anhydride, then remaining dithiocarbonic anhydride is reclaimed in underpressure distillation, obtains simultaneously xanthogenate.
Solvent dithiocarbonic anhydride of the present invention, itself be also the raw material of producing xanthogenate, and its ratio with the consumption of another kind of raw alcohol is 3～9: 1 (ratio of amount of substance).Because dithiocarbonic anhydride is excessive more than 2 times, produce in the xanthogenate process and stir fully, caustic alkali (sodium hydroxide or potassium hydroxide) can be sheet alkali or grain alkali or powder alkali, the fine dispersion of the xanthogenate of caustic alkali and generation energy in reaction process, the heat energy that reaction is emitted is removed in time, temperature of reaction is controlled, thus the yield of xanthogenate product and purity high.The present invention also be take nitrogen as the reaction shielding gas, and dithiocarbonic anhydride and air are isolated fully, stops its steam and air to form explosive mixture, stops its burning, greatly reduces the volatilization loss of dithiocarbonic anhydride.In addition, because the boiling point of dithiocarbonic anhydride is low, be only 46.5 ℃, the low advantage of required energy consumption during Distillation recovery.
Therefore, the present invention adopts substep under nitrogen protection to pass through the excessive dithiocarbonic anhydride of Distillation recovery, and the loss of dithiocarbonic anhydride is extremely low.The boiling point of dithiocarbonic anhydride is low, is only 46.5 ℃, and during Distillation recovery, energy consumption is low; During underpressure distillation, part water also can be with the steaming and take out of of dithiocarbonic anhydride, and the solubleness of water in dithiocarbonic anhydride is extremely low, and the density of dithiocarbonic anhydride is greater than again water, be easy to realize separating of dithiocarbonic anhydride and water, dithiocarbonic anhydride is easily realized recycle and can not had a negative impact to production; And, by regulating vacuum distillation temperature, time or pressure, can obtain the controlled xanthate product of xanthogenate content (84%～96%).
Preferred alcohols of the present invention: dithiocarbonic anhydride: the ratio of the amount of substance of caustic alkali is 1: 3～6: 1～1.05 situation, but the feed stock conversion of reaction De Genggaogengjia; More be conducive to the highly effective reaction that economizes in raw materials, and the follow-up recycling to dithiocarbonic anhydride, and cost-saving.
The present invention, under 10 ℃～70 ℃ of temperature of reaction, continues reaction 0.5～8 hour.
Described caustic alkali is sodium hydroxide or potassium hydroxide, is Powdered or particulate state or sheet.
Describedly under nitrogen protection, be filtered into the nitrogen press filtration.
The present invention preferably under 5 ℃～35 ℃ whipped states, add alcohol, caustic alkali in another kind in two kinds; Under 20 ℃～35 ℃, continue reaction, the reaction times is 3～5 hours.
The concrete embodiment of the present invention is::
In reactor, add alcohol and dithiocarbonic anhydride, the ratio of both amount of substances is n (alcohol): n (dithiocarbonic anhydride)=1: 3～9, stir and 0 ℃～40 ℃ under add caustic alkali (sodium hydroxide or potassium hydroxide) in batches, add-on is n (alcohol): n (caustic alkali)=1: 1～1.1 (ratios of amount of substance), adding after alkali is to react 0.5～8 hour under 10 ℃～70 ℃ in temperature of reaction again, generates xanthogenate.
Or in reactor, add caustic alkali (sodium hydroxide or potassium hydroxide) and dithiocarbonic anhydride, the ratio of both amount of substances is n (caustic alkali): n (dithiocarbonic anhydride)=1: 3～9, stir and 0 ℃～40 ℃ under add alcohol, add-on is n (alcohol): n (alkali)=1: 1～1.1 (ratios of amount of substance), adding after alcohol is to react 0.5～8 hour under 10 ℃～70 ℃ in temperature of reaction again, generates xanthogenate.
Reaction equation is:
Wherein R-OH is potato spirit, C
2-C
8Fatty alcohol in one or more, be preferably one or more in ethanol, propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, sec-butyl alcohol, amylalcohol, primary isoamyl alcohol, sec.-amyl alcohol, neopentyl alcohol, n-hexyl alcohol, isohexyl alcohol, secondary hexyl alcohol, methyl isobutyl carbinol, n-Octanol, secondary octanol, isooctyl alcohol, potato spirit.M is Na or K; In industrial production, reaction process be take nitrogen and is shielding gas.
The mode that the excessive reaction solvent dithiocarbonic anhydride of the present invention reclaims is: mode one is that reactor reaction mixture is out filtered under nitrogen protection, and the filter cake underpressure distillation obtains respectively xanthogenate product and the dithiocarbonic anhydride solvent of (high purity); The dithiocarbonic anhydride of filtrate and recovery recycles.Mode two is after first with nitrogen replacement, falling the air in distillation plant, reactor reaction mixture out is first 50 ℃～90 ℃ lower air distillations, reclaim most dithiocarbonic anhydride, then remaining dithiocarbonic anhydride is reclaimed in underpressure distillation, obtains simultaneously the controlled xanthate product of xanthogenate content (84%～96%).
The preferred filter type of the present invention is the nitrogen press filtration.Preferred air distillation temperature is 70 ℃～80 ℃.Preferred normal pressure, vacuum distillation equipment are rake type drier.
Embodiment
The present invention is further illustrated by following examples, but is not subjected to the restriction of these embodiment.In embodiment, all umbers and percentage ratio go out separately to have regulation all to refer to quality outward.
The preparation of reference examples 1 sodium isobutyl xanthan
According to the method that the people such as M.Alijanianzadeh provide, synthesize sodium isobutyl xanthan (M.Alijanianzadeh, A.A.Saboury, H.Mansuri-torshizi, K.Haghbeen, A.A.Moosavi-movahedi.The inhibitory effect of some new synthesized xanthates on mushroom tyrosinase activities[J] .Journal of Enzyme Inhibition and Medicinal Chemistry, 2007,22 (2): 239-246.).
By 14.98 parts of purity, be that 99% isopropylcarbinol and 5.81 parts of purity are that 96% Powdered sodium hydroxide adds in reactor, fully stir; Then reactor is cooling with frozen water, in 30 minutes, adding 30.75 parts of purity is 99% dithiocarbonic anhydride (ratio of the amount of substance of alcohol and dithiocarbonic anhydride be n (alcohol): n (dithiocarbonic anhydride)=1: 2), after adding dithiocarbonic anhydride, continuation is the cooling lower stirring reaction of frozen water 1 hour, then stirring at room reaction 2 hours.In reaction process, stir more and more difficultly, in final reactor, cannot see liquid, material almost becomes dry, and in thick product, a large amount of punctations is arranged, and is unreacted sodium hydroxide.After the dithiocarbonic anhydride in thick product was taken off in decompression, in product, sodium isobutyl xanthan purity was 84.1% by analysis, was 85.3% based on the product yield of isopropylcarbinol.
The preparation of embodiment 2 sodium isobutyl xanthans
By 46.13 parts of purity, be that 99% dithiocarbonic anhydride and 14.98 parts of purity are that 99% isopropylcarbinol adds in reactor (ratio of the amount of substance of alcohol and dithiocarbonic anhydride be n (alcohol): n (dithiocarbonic anhydride)=1: 3), under agitation by the cooling 15 ℃ of left and right of this mixture, then divide 3 times, being respectively 3 parts, 3 parts and 2.34 parts of flaky sodium hydrates (purity is 96%) is added in reactor, add rear stirring about 10 minutes at every turn, temperature when control alkali is reinforced is 15 ℃～30 ℃, after adding caustic alkali, 25 ℃ of stirring reactions 2 hours, reaction finished.By the first normal pressure of excessive dithiocarbonic anhydride solvent, decompression substep Distillation recovery again, obtain needed sodium isobutyl xanthan product.The analysis showed that sodium isobutyl xanthan purity is 88.9%, is 95.4% based on the product yield of isopropylcarbinol.
The preparation of embodiment 3 sodium isobutyl xanthans
The dithiocarbonic anhydride and the 8.34 parts of granular sodium hydroxide (purity is 96%) that by 46.13 parts of purity, are 99% add in reactor, under agitation this mixture is cooled to 15 ℃ of left and right, then 15 ℃～30 ℃ and stir under use that to reactor, to drip 14.98 parts of purity be 99% isopropylcarbinol (ratio of the amount of substance of alcohol and dithiocarbonic anhydride be n (alcohol): n (dithiocarbonic anhydride)=1: 3), dripping the maintenance temperature of reaction is 25 ℃, stirring reaction 4 hours, reaction finishes.By the first normal pressure of excessive dithiocarbonic anhydride solvent, decompression substep Distillation recovery again, obtain needed sodium isobutyl xanthan product.The analysis showed that sodium isobutyl xanthan purity is 89.2%, is 96.8% based on the product yield of isopropylcarbinol.
The preparation of embodiment 4 sodium isobutyl xanthans
It is 61.50 parts of dithiocarbonic anhydride (ratios of alcohol and the amount of substance of dithiocarbonic anhydride be n (alcohol): n (dithiocarbonic anhydride)=1: 4) that 46.13 parts of dithiocarbonic anhydride in embodiment 2 are used instead, granular sodium hydroxide (purity is 96%) is used instead as flaky sodium hydrate, other conditions are constant, in the sodium isobutyl xanthan product obtained, the purity of sodium isobutyl xanthan is 88.4%, is 97.1% based on the product yield of isopropylcarbinol.
The preparation of embodiment 5 sodium n-butyl xanthates
Isopropylcarbinol in embodiment 1 is used instead as butanols, and other conditions are constant, and in the sodium n-butyl xanthate product obtained, sodium n-butyl xanthate purity is 88.7%, are 95.9% based on the product yield of propyl carbinol.
The preparation of embodiment 6 isopentyl sodium xanthonates
By 14.98 parts of purity in embodiment 2, be that 99% isopropylcarbinol replaces with the primary isoamyl alcohol that 17.90 parts of purity are 99%, other conditions are constant, in the isopentyl sodium xanthonate product obtained, isopentyl sodium xanthonate purity is 85.6%, is 92.4% based on the product yield of primary isoamyl alcohol.
The preparation of embodiment 7 methyl-isobutyl methyl sodium xanthonates
By 14.98 parts of purity in embodiment 1, be that 99% isopropylcarbinol is that 21.16 parts of purity are 99% methyl isobutyl carbinol with using instead, other conditions are constant, in the methyl-isobutyl methyl sodium xanthonate product obtained, methyl-isobutyl methyl sodium xanthonate purity is 84.3%, is 89.6% based on the product yield of methyl isobutyl carbinol.
The preparation of embodiment 8 secondary octyl sodium xanthonates
By 14.98 parts of purity in embodiment 1, be that 99% isopropylcarbinol is that 26.29 parts of purity are 99% secondary octanol with using instead, other conditions are constant, in the secondary octyl sodium xanthonate product obtained, secondary octyl sodium xanthonate purity is 84.2%, is 86.6% based on the product yield of secondary octanol.
The preparation of embodiment 9 Isobutylxanthic acids and methyl-isobutyl methyl xanthate mixing xanthate
By 14.98 parts of purity in embodiment 1, be 99% isopropylcarbinol be that 7.49 parts of purity are that 99% isopropylcarbinol and 10.58 parts of purity are 99% methyl isobutyl carbinol with using instead, other conditions are constant, in the Isobutylxanthic acid obtained and methyl-isobutyl methyl xanthate mixing xanthate product, mixing xanthate purity is 84.8%, is 95.6% based on the product yield of sodium hydroxide.
The preparation of embodiment 10 sodium isobutyl xanthans
First with nitrogen, the air in reactor is caught up with totally, then to adding 756 parts of purity in reactor, be 99% dithiocarbonic anhydride, adding 150 parts of purity is 99% isopropylcarbinol (ratio of the amount of substance of alcohol and dithiocarbonic anhydride be n (alcohol): n (dithiocarbonic anhydride)=1: 4.9) again, under agitation by 83.4 parts of flaky sodium hydrates (purity is 96%), dividing many batches joins in reactor, controlling temperature of reaction kettle while feeding in raw material is 10 ℃～32 ℃, after adding alkali, keep 20 ℃～35 ℃ of temperature of reaction kettle, stirring reaction is 4 hours again, and reaction finishes.With nitrogen, the rake type drier Air is replaced; then the material in reactor is introduced to rake type drier under nitrogen protection; with 80 ℃ of hot water, heat up; the dithiocarbonic anhydride as solvent is reclaimed in air distillation; when the dithiocarbonic anhydride flow got off when condensation in condenser is very little; stop air distillation, push back test tank with the dithiocarbonic anhydride that nitrogen reclaims air distillation.Then open underpressure distillation and reclaim remaining dithiocarbonic anhydride, during underpressure distillation, progressively increase vacuum tightness, until vacuum tightness reach 0.06MPa～-0.1MPa, stop underpressure distillation, needed sodium isobutyl xanthan product is in rake type drier.The analysis showed that sodium isobutyl xanthan purity is 89.6%, is 95.4% based on the yield of isopropylcarbinol.
The preparation of embodiment 11 sodium isobutyl xanthans
First with nitrogen, the air in reactor is caught up with totally, then to adding 600 parts of purity in reactor, be 99% dithiocarbonic anhydride, adding 150 parts of purity is 99% isopropylcarbinol (ratio of the amount of substance of alcohol and dithiocarbonic anhydride be n (alcohol): n (dithiocarbonic anhydride)=1: 3.9) again, under agitation by 83.4 parts of flaky sodium hydrates (purity is 96%), dividing many batches joins in reactor, controlling temperature of reaction kettle while feeding in raw material is 10 ℃～32 ℃, after adding alkali, keep 20 ℃～35 ℃ of temperature of reaction kettle, stirring reaction is 5 hours again, and reaction finishes.With nitrogen, by the displacement of full automatic pressure filter Air, then the material in reactor is introduced under nitrogen protection to this full automatic pressure filter, used the nitrogen press filtration, filtrate is returned to test tank for reaction next time.Filter cake enters and with nitrogen replacement, falls in the rake type drier of air in advance, with 60 ℃ of hot water, heat up, open underpressure distillation and reclaim remaining dithiocarbonic anhydride, during underpressure distillation, progressively increase vacuum tightness, until vacuum tightness reach 0.06MPa～-0.1MPa, stop underpressure distillation, needed sodium isobutyl xanthan product is in rake type drier.The analysis showed that sodium isobutyl xanthan purity is 90.5%, is 94.5% based on the yield of isopropylcarbinol.
Claims (9)
1. the synthetic method of an xanthogenate, it is characterized in that, the dithiocarbonic anhydride of take is reaction raw materials and solvent, the nitrogen of take is the reaction shielding gas, add a kind of in two kinds of reaction raw materials alcohol, caustic alkali, another kind add two kinds of reaction raw materials alcohol, caustic alkali under 0 ℃～40 ℃ whipped states in is under 10 ℃～70 ℃, to continue reaction in temperature of reaction; After having reacted, from reaction mixture, isolating excessive dithiocarbonic anhydride, thereby obtain xanthogenate; Described alcohol: dithiocarbonic anhydride: the ratio of the amount of substance of caustic alkali is 1:3～9:1～1.1; Described alcohol is potato spirit, C
2-C
8Fatty alcohol in one or more.
2. synthetic method according to claim 1, is characterized in that, alcohol: dithiocarbonic anhydride: the ratio of the amount of substance of caustic alkali is 1:3～6:1～1.05.
3. synthetic method according to claim 1, is characterized in that, under 10 ℃～70 ℃ of temperature of reaction, continues reaction 0.5～8 hour.
4. synthetic method according to claim 1, it is characterized in that, described alcohol is selected from as one or more in ethanol, propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, sec-butyl alcohol, amylalcohol, primary isoamyl alcohol, sec.-amyl alcohol, neopentyl alcohol, n-hexyl alcohol, isohexyl alcohol, secondary hexyl alcohol, methyl isobutyl carbinol, n-Octanol, secondary octanol, isooctyl alcohol, potato spirit.
5. synthetic method according to claim 1, is characterized in that, described caustic alkali is sodium hydroxide or potassium hydroxide, is Powdered or particulate state or sheet.
6. synthetic method according to claim 1, is characterized in that, the another kind add two kinds of reaction raw materials alcohol, caustic alkali under 5 ℃～35 ℃ whipped states in; Under 20 ℃～35 ℃, continue reaction, the reaction times is 3～5 hours.
7. according to the described synthetic method of claim 1-6 any one, it is characterized in that, described to isolate excessive dithiocarbonic anhydride be that reaction mixture is filtered under nitrogen protection, and the filter cake underpressure distillation, obtain respectively xanthogenate and dithiocarbonic anhydride; Or after first with nitrogen replacement, falling the air in distillation plant, reaction mixture, first 50 ℃～90 ℃ lower air distillations, is reclaimed to dithiocarbonic anhydride, then remaining dithiocarbonic anhydride is reclaimed in underpressure distillation.
8. synthetic method according to claim 7, is characterized in that, describedly under nitrogen protection, is filtered into the nitrogen press filtration.
9. synthetic method according to claim 7, is characterized in that, the air distillation temperature is 70 ℃～80 ℃.
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| CN104774166A (en) * | 2015-04-28 | 2015-07-15 | 兰州泰顺科技有限公司 | Synthetic method for disulfide diisopropyl xanthate |
| CN107235879A (en) * | 2017-05-23 | 2017-10-10 | 西北矿冶研究院 | Synthesis process of liquid xanthate |
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| CN107824340A (en) * | 2017-11-30 | 2018-03-23 | 广东省资源综合利用研究所 | A kind of preparation method and application of noble metal collecting agent |
| CN108569989B (en) | 2018-05-25 | 2020-06-02 | 中南大学 | Method for preparing thiourethane and co-producing 2-mercaptoethanol or O-alkylthio ethyl xanthate |
| CN111195513A (en) * | 2020-02-14 | 2020-05-26 | 兰州交通大学 | Preparation method of dithio-carboxylated straw, product and application of product as heavy metal adsorbent |
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