CN102690218A - Method for synthesizing xanthate - Google Patents
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- CN102690218A CN102690218A CN2012101273613A CN201210127361A CN102690218A CN 102690218 A CN102690218 A CN 102690218A CN 2012101273613 A CN2012101273613 A CN 2012101273613A CN 201210127361 A CN201210127361 A CN 201210127361A CN 102690218 A CN102690218 A CN 102690218A
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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) is commonly called as " xanthate ", can form with multiple metals ion to dissolve compound.1815, the synthetic first xanthogenate of Cai Si (Zeise) was because it is yellow, so 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 maximum sulfide flotation collector of mineral manufacture field consumption.
At present, the method for synthetic xanthate mainly contains " kneading method " and " solvent method ".Kneading method is that pure and mild dithiocarbonic anhydride is added kneading machine, progressively adds powder alkali (sodium hydroxide or Pottasium Hydroxide) then, 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 working method (Tian Xishuan, Wang Yongxin. the xanthate working 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 this method need be made the alkali system sheet alkali or granulated alkali are pulverized, and powder alkali water absorbability and corrodibility are strong.This method needs raw material fully to mix to pinch simultaneously, strict control reaction temperature, 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 influences the quality of xanthate product.
Solvent method is that alcohol, dithiocarbonic anhydride and alkali are reacted in certain amount of solvent, steams to desolventize after having reacted to obtain the xanthate product.Solvent method need not made the alkali system; And chemical reaction carries out in liquid phase all the time; Sodium hydroxide that adds in the process or Pottasium Hydroxide are easy to scatter, and simultaneously solvent can in time be removed reaction heat, have avoided producing because of local superheating the shortcoming that impurity such as inorganic sulphide and non-xanthate organic sulfide cause poor product quality; Thereby the transformation efficiency of alcohol is high, and the yield of xanthate and purity are also high.There is the solvent of report to mainly contain (Shi Xianyi such as benzene, toluene, kerosene, ethylene dichloride, raw alcohol, YLENE, ethylbenzene, gasoline at present; Qin Xuemei; Deng Zhongyan. the improvement of Synthesis Process of Sodium n-butyl Xanthate [J]. chemical industry 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 working 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).Whether according to solvent is reaction raw materials, can solvent method be divided into non-raw material solvent method and alcohol excess method again.Wherein non-raw material solvent method needs to prepare nonreactants such as introducing benzene, toluene, kerosene, ethylene dichloride, YLENE, ethylbenzene or gasoline in the process at xanthate; Can dithiocarbonic anhydride or raw alcohol be brought in the non-raw material solvent together completely with the part unreacted during desolventizing; The metering of dithiocarbonic anhydride or raw alcohol can not be accurate when causing down secondary response, influences 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 that generates 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 the direct circulation of alcohol will be introduced water when descending secondary response, has a strong impact on xanthate quality product and yield; And pure boiling point is higher, and the solvent recuperation energy consumption is higher.So solvent method is seldom adopted by industrial production.
2007; M.Alijanianzadeh etc. have reported that the 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, is well on when beginning to react; But reaction late phase reaction material becomes dry fully; Stir difficulty, for this reason, they add acetone solvent so that stir smoothly.Because contain dithiocarbonic anhydride and solvent acetone in the reaction mixture, they do not reclaim excessive dithiocarbonic anhydride raw material, 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 compound 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 easy realization of industrial cyclic production more.
Further object of the present invention is, provides a kind of simple and convenient, can the efficient recovery of the excessive dithiocarbonic anhydride that produces in the above-mentioned compound method be separated the method for recycling.
Technical scheme of the present invention is: be reaction raw materials and solvent with dithiocarbonic anhydride; With nitrogen is the reaction shielding gas; Add in reaction raw materials alcohol, the caustic alkali a kind of in two kinds; Under 0 ℃～40 ℃ whipped states, add the another kind in two kinds in alcohol, the caustic alkali, be 10 ℃～70 ℃ in temperature of reaction and continue reaction down; Reaction is isolated excessive dithiocarbonic anhydride after accomplishing from reaction mixture, 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(C12-C14 and C12-C18).
Describedly isolate excessive dithiocarbonic anhydride, reaction mixture is filtered under nitrogen protection, the filter cake underpressure distillation obtains xanthogenate and dithiocarbonic anhydride respectively; Or after falling the air in the distillation plant with nitrogen replacement earlier, reaction mixture earlier 50 ℃～90 ℃ following air distillations, reclaiming dithiocarbonic anhydride, remaining dithiocarbonic anhydride is reclaimed in underpressure distillation then, obtains xanthogenate simultaneously.
The solvent dithiocarbonic anhydride that the present invention adopted itself also is 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 and stir in the xanthogenate process fully; Caustic alkali (sodium hydroxide or Pottasium Hydroxide) can be sheet alkali or grain alkali or powder alkali, the xanthogenate of caustic alkali and generation ability well dispersed in the reaction process, and the heat energy that reaction is emitted is in time removed; Temperature of reaction is controlled, thereby the yield of xanthogenate product and purity height.The present invention also is the reaction shielding gas with nitrogen, 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,, be merely 46.5 ℃, the low advantage of required energy consumption when distillation is reclaimed because the boiling point of dithiocarbonic anhydride is low.
Therefore, the present invention adopts under the nitrogen protection and reclaims excessive dithiocarbonic anhydride through distillation step by step, and the loss of dithiocarbonic anhydride is extremely low.The boiling point of dithiocarbonic anhydride is low, is merely 46.5 ℃, and energy consumption was low when distillation was reclaimed; During underpressure distillation; Portion 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 again greater than water; Be easy to realize separating of dithiocarbonic anhydride and water that dithiocarbonic anhydride is realized recycle easily and can production do not had a negative impact; And, can obtain the controlled xanthate product of xanthogenate content (84%～96%) through regulating vacuum distillation temperature, time or pressure.
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 help the highly effective reaction that economizes in raw materials, and the follow-up recycling to dithiocarbonic anhydride, and practice thrift cost.
The present invention continues reaction 0.5～8 hour under 10 ℃～70 ℃ of temperature of reaction.
Described caustic alkali is sodium hydroxide or Pottasium Hydroxide, is Powdered or particulate state or sheet.
Describedly under nitrogen protection, be filtered into the nitrogen press filtration.
The present invention preferably adds the another kind in two kinds in alcohol, the caustic alkali under 5 ℃～35 ℃ whipped states; Continue reaction down at 20 ℃～35 ℃, the reaction times is 3～5 hours.
The concrete embodiment of the present invention is::
In reaction kettle, add pure and mild 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 Pottasium Hydroxide) in batches; Add-on is n (alcohol): n (caustic alkali)=1: 1～1.1 (ratios of amount of substance), and adding behind the alkali in temperature of reaction is to react 0.5～8 hour under 10 ℃～70 ℃ again, generates xanthogenate.
Or in reaction kettle, add caustic alkali (sodium hydroxide or Pottasium Hydroxide) and dithiocarbonic anhydride; The ratio of both amount of substances is n (caustic alkali): n (dithiocarbonic anhydride)=1: 3～9; Stirring and 0 ℃～40 ℃ following alcohol that add; Add-on is n (alcohol): n (alkali)=1: 1～1.1 (ratios of amount of substance), and adding the alcohol back 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(C12-C14 and C12-C18) in one or more, be preferably 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, the potato spirit one or more.M is Na or K; Reaction process is shielding gas with nitrogen in the industrial production.
The mode that the excessive reaction solvent dithiocarbonic anhydride of the present invention reclaims is: mode one is that the reaction mixture that reaction kettle comes out is filtered under nitrogen protection, and the filter cake underpressure distillation obtains the xanthogenate product and the dithiocarbonic anhydride solvent of (high purity) respectively; Filtrating and the dithiocarbonic anhydride that reclaims recycle.Mode two is after falling the air in the distillation plant with nitrogen replacement earlier; The reaction mixture that reaction kettle comes out is first 50 ℃～90 ℃ following air distillations; Reclaim most dithiocarbonic anhydride; Remaining dithiocarbonic anhydride is reclaimed in underpressure distillation then, obtains the controlled xanthate product of xanthogenate content (84%～96%) simultaneously.
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 specified by following examples, but does not receive the restriction of these embodiment.All umbers and percentage ratio go out to have in addition regulation all to refer to quality outward among the embodiment.
The preparation of reference examples 1 sodium isobutyl xanthan
Method according to people such as M.Alijanianzadeh provide is synthesized 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.).
With 14.98 parts of purity is that 99% isopropylcarbinol and 5.81 parts of purity are that 96% Powdered sodium hydroxide adds in the reactor drum, fully stirs; Then reactor drum is cooled off with frozen water; In 30 minutes, add 30.75 parts of purity and be 99% dithiocarbonic anhydride (ratio of the amount of substance of pure and mild dithiocarbonic anhydride be n (alcohol): n (dithiocarbonic anhydride)=1: 2); After adding dithiocarbonic anhydride; Continuation was reacted 2 hours in stirring at room at frozen water cooling stirring reaction 1 hour down then.Stir more and more difficult in the reaction process, cannot see liquid in the final reactor, material almost becomes dry, and in the thick product a large amount of punctations is arranged, and is unreacted sodium hydroxide.After the dithiocarbonic anhydride in the thick product was taken off in decompression, sodium isobutyl xanthan purity was 84.1% in analysed preparation, was 85.3% based on the product yield of isopropylcarbinol.
The preparation of embodiment 2 sodium isobutyl xanthans
With 46.13 parts of purity is that 99% dithiocarbonic anhydride and 14.98 parts of purity are that 99% isopropylcarbinol adds in the reactor drum (ratio of the amount of substance of pure and mild dithiocarbonic anhydride be n (alcohol): n (dithiocarbonic anhydride)=1: 3); Under agitation with about 15 ℃ of this mixture coolings; Divide then 3 times, be respectively 3 parts, 3 parts and 2.34 parts of flaky sodium hydrates (purity is 96%) and be added in the reactor drum, add the back at every turn and stirred about 10 minutes; Temperature when control alkali is reinforced is 15 ℃～30 ℃; After adding caustic alkali, 25 ℃ of stirring reactions 2 hours, reaction finished.With the first normal pressure of excessive dithiocarbonic anhydride solvent, decompression substep distillation recovery again, obtain needed sodium isobutyl xanthan product.Analysis revealed 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
With 46.13 parts of purity is that 99% dithiocarbonic anhydride and 8.34 parts of granular sodium hydroxide (purity is 96%) add in the reactor drum; Under agitation this mixture is cooled to about 15 ℃; Then 15 ℃～30 ℃ with stir that to use to 14.98 parts of purity of reactor drum dropping down be 99% isopropylcarbinol (ratio of the amount of substance of pure and mild dithiocarbonic anhydride as n (alcohol): n (dithiocarbonic anhydride)=1: 3); Dripping the maintenance temperature of reaction is 25 ℃, stirring reaction 4 hours, and reaction finishes.With the first normal pressure of excessive dithiocarbonic anhydride solvent, decompression substep distillation recovery again, obtain needed sodium isobutyl xanthan product.Analysis revealed 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 the amount of substance of pure and mild dithiocarbonic anhydride be n (alcohol): n (dithiocarbonic anhydride)=1: 4) that 46.13 parts of dithiocarbonic anhydride among the embodiment 2 are used instead; Granular sodium hydroxide (purity is 96%) is used instead and is flaky sodium hydrate; Other conditions are constant; The purity of sodium isobutyl xanthan is 88.4% in the sodium isobutyl xanthan product that obtains, and is 97.1% based on the product yield of isopropylcarbinol.
The preparation of embodiment 5 sodium n-butyl xanthates
Isopropylcarbinol among the embodiment 1 used instead be butanols, other conditions are constant, and sodium n-butyl xanthate purity is 88.7% in the sodium n-butyl xanthate product that obtains, and are 95.9% based on the product yield of propyl carbinol.
The preparation of embodiment 6 isopentyl sodium xanthonates
With 14.98 parts of purity among the embodiment 2 is that to use 17.90 parts of purity be that 99% primary isoamyl alcohol replaces for 99% isopropylcarbinol; Other conditions are constant; Isopentyl sodium xanthonate purity is 85.6% in the isopentyl sodium xanthonate product that obtains, and is 92.4% based on the product yield of primary isoamyl alcohol.
The preparation of embodiment 7 methyl-isobutyl methyl sodium xanthonates
With 14.98 parts of purity among the embodiment 1 is that 99% isopropylcarbinol uses that to use instead be that 21.16 parts of purity are 99% methyl isobutyl carbinol; Other conditions are constant; Methyl-isobutyl methyl sodium xanthonate purity is 84.3% in the methyl-isobutyl methyl sodium xanthonate product that obtains, and is 89.6% based on the product yield of methyl isobutyl carbinol.
The preparation of embodiment 8 secondary octyl sodium xanthonates
With 14.98 parts of purity among the embodiment 1 is that 99% isopropylcarbinol uses that to use instead be that 26.29 parts of purity are 99% secondary octanol; Other conditions are constant; Secondary octyl sodium xanthonate purity is 84.2% in the secondary octyl sodium xanthonate product that obtains, and is 86.6% based on the product yield of secondary octanol.
The preparation of embodiment 9 Isobutylxanthic acids and methyl-isobutyl methyl xanthate mix yellow medicine
With 14.98 parts of purity among the embodiment 1 is that 99% isopropylcarbinol uses that to use instead be that 7.49 parts of purity are that 99% isopropylcarbinol and 10.58 parts of purity are 99% methyl isobutyl carbinol; Other conditions are constant; Mixing xanthate purity in the Isobutylxanthic acid that obtains and the methyl-isobutyl methyl xanthate mix yellow medicine product is 84.8%, is 95.6% based on the product yield of sodium hydroxide.
The preparation of embodiment 10 sodium isobutyl xanthans
With nitrogen the air in the reaction kettle is caught up with totally earlier; In reaction kettle, add 756 parts of purity then and be 99% dithiocarbonic anhydride; Add 150 parts of purity again and be 99% isopropylcarbinol (ratio of the amount of substance of pure and mild dithiocarbonic anhydride be n (alcohol): n (dithiocarbonic anhydride)=1: 4.9), under agitation divide many batches with 83.4 parts of flaky sodium hydrates (purity is 96%) and join in the reaction kettle, temperature of reaction kettle was 10 ℃～32 ℃ when control was reinforced; After adding alkali; Keep 20 ℃～35 ℃ of temperature of reaction kettle, restir reaction 4 hours, reaction finishes.With nitrogen the rake type drier air is replaced; Then the material in the reaction kettle is introduced rake type drier under nitrogen protection; Heat up with 80 ℃ of hot water, the dithiocarbonic anhydride as solvent is reclaimed in air distillation, when the dithiocarbonic anhydride flow that gets off when condensation in the condensing surface is very little; Stop air distillation, the dithiocarbonic anhydride that air distillation is reclaimed with nitrogen pushes back test tank.Open underpressure distillation then and reclaim remaining dithiocarbonic anhydride, progressively increase vacuum tightness during underpressure distillation, until vacuum tightness reach 0.06MPa～-0.1MPa, stop underpressure distillation, needed sodium isobutyl xanthan product is in rake type drier.Analysis revealed sodium isobutyl xanthan purity is 89.6%, is 95.4% based on the yield of isopropylcarbinol.
The preparation of embodiment 11 sodium isobutyl xanthans
With nitrogen the air in the reaction kettle is caught up with totally earlier; In reaction kettle, add 600 parts of purity then and be 99% dithiocarbonic anhydride; Add 150 parts of purity again and be 99% isopropylcarbinol (ratio of the amount of substance of pure and mild dithiocarbonic anhydride be n (alcohol): n (dithiocarbonic anhydride)=1: 3.9), under agitation divide many batches with 83.4 parts of flaky sodium hydrates (purity is 96%) and join in the reaction kettle, temperature of reaction kettle was 10 ℃～32 ℃ when control was reinforced; After adding alkali; Keep 20 ℃～35 ℃ of temperature of reaction kettle, restir reaction 5 hours, reaction finishes.With the displacement of full automatic pressure filter air, then the material in the reaction kettle is introduced this full automatic pressure filter with nitrogen under nitrogen protection, use the nitrogen press filtration, filtrating is returned test tank and is used for reacting next time.Filter cake gets into to fall in the rake type drier of air with nitrogen replacement in advance; Heat up with 60 ℃ of hot water; Open underpressure distillation and reclaim remaining dithiocarbonic anhydride, progressively increase vacuum tightness during underpressure distillation, until vacuum tightness reach 0.06MPa～-0.1MPa; Stop underpressure distillation, needed sodium isobutyl xanthan product is in rake type drier.Analysis revealed sodium isobutyl xanthan purity is 90.5%, is 94.5% based on the yield of isopropylcarbinol.
Claims (9)
1. the compound method of an xanthogenate; It is characterized in that; With dithiocarbonic anhydride is reaction raw materials and solvent, is the reaction shielding gas with nitrogen, adds in reaction raw materials alcohol, the caustic alkali a kind of in two kinds; Under 0 ℃～40 ℃ whipped states, add the another kind in two kinds in alcohol, the caustic alkali, be 10 ℃～70 ℃ in temperature of reaction and continue reaction down; Reaction is isolated excessive dithiocarbonic anhydride, thereby is obtained xanthogenate after accomplishing from reaction mixture; 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(C12-C14 and C12-C18) in one or more.
2. compound 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. compound method according to claim 1 is characterized in that, continues reaction 0.5～8 hour down for 10 ℃～70 ℃ in temperature of reaction.
4. compound method according to claim 1; It is characterized in that said alcohol is selected from and is 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, the potato spirit one or more.
5. compound method according to claim 1 is characterized in that, described caustic alkali is sodium hydroxide or Pottasium Hydroxide, is Powdered or particulate state or sheet.
6. compound method according to claim 1 is characterized in that, under 5 ℃～35 ℃ whipped states, adds the another kind in two kinds in alcohol, the caustic alkali; Continue reaction down at 20 ℃～35 ℃, the reaction times is 3～5 hours.
7. according to each described compound method of claim 1-6, it is characterized in that described to isolate excessive dithiocarbonic anhydride be that reaction mixture is filtered under nitrogen protection, the filter cake underpressure distillation obtains xanthogenate and dithiocarbonic anhydride respectively; Or after falling the air in the distillation plant with nitrogen replacement earlier, reaction mixture earlier 50 ℃～90 ℃ following air distillations, reclaiming dithiocarbonic anhydride, remaining dithiocarbonic anhydride is reclaimed in underpressure distillation then.
8. compound method according to claim 1 is characterized in that, describedly under nitrogen protection, is filtered into the nitrogen press filtration.
9. compound method according to claim 1 is characterized in that, the air distillation temperature is 70 ℃～80 ℃.
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| CN103304461A (en) * | 2013-06-14 | 2013-09-18 | 紫金矿业集团股份有限公司 | Synthesis and preparation method of gold-containing sulphide ore collecting agent compound |
| CN103817014A (en) * | 2014-02-21 | 2014-05-28 | 中南大学 | Preparation method for granular xanthate |
| 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 |
| CN107737672A (en) * | 2017-09-28 | 2018-02-27 | 四川有色金砂选矿药剂有限公司 | Ore dressing xanthate and preparation method thereof |
| 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 |
| CN108569989A (en) * | 2018-05-25 | 2018-09-25 | 中南大学 | A method of preparing thiourethane co-production 2 mercapto ethanol or O- alkylthio group ethyl xanthates |
| WO2019223290A1 (en) * | 2018-05-25 | 2019-11-28 | 中南大学 | Method for preparing thiourethane and producing 2-mercaptoethanol or o-alkyl ethyl xanthate in parallel |
| US11970441B2 (en) | 2018-05-25 | 2024-04-30 | Central South University | Method for preparing thionocarbamate and co-producing 2-mercaptoethanol or O-alkylthioethyl 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 |
| CN111606832A (en) * | 2020-06-30 | 2020-09-01 | 陕西华光实业有限责任公司 | Production method of high-grade potassium xanthate |
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