CN116283687A - Synthesis process of diisoamyl sulfide - Google Patents
Synthesis process of diisoamyl sulfide Download PDFInfo
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- CN116283687A CN116283687A CN202211091854.6A CN202211091854A CN116283687A CN 116283687 A CN116283687 A CN 116283687A CN 202211091854 A CN202211091854 A CN 202211091854A CN 116283687 A CN116283687 A CN 116283687A
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- JWEWNTJADCWFRP-UHFFFAOYSA-N 3-methyl-1-(3-methylbutylsulfanyl)butane Chemical compound CC(C)CCSCCC(C)C JWEWNTJADCWFRP-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 28
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 17
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000010992 reflux Methods 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 16
- YXZFFTJAHVMMLF-UHFFFAOYSA-N 1-bromo-3-methylbutane Chemical compound CC(C)CCBr YXZFFTJAHVMMLF-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000004821 distillation Methods 0.000 claims abstract description 15
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 23
- 235000019441 ethanol Nutrition 0.000 claims description 15
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 6
- 159000000000 sodium salts Chemical class 0.000 claims description 6
- 238000004817 gas chromatography Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 238000005292 vacuum distillation Methods 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical class CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 claims 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 abstract description 43
- 229910052763 palladium Inorganic materials 0.000 abstract description 22
- 238000000605 extraction Methods 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000011541 reaction mixture Substances 0.000 abstract 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 4
- IUGROBBTJKXBHX-UHFFFAOYSA-N 2-methylbutane hydrobromide Chemical compound Br.CCC(C)C IUGROBBTJKXBHX-UHFFFAOYSA-N 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 2
- 239000001639 calcium acetate Substances 0.000 description 2
- 235000011092 calcium acetate Nutrition 0.000 description 2
- 229960005147 calcium acetate Drugs 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- 235000012255 calcium oxide Nutrition 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000658 coextraction Methods 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C321/00—Thiols, sulfides, hydropolysulfides or polysulfides
- C07C321/12—Sulfides, hydropolysulfides, or polysulfides having thio groups bound to acyclic carbon atoms
- C07C321/14—Sulfides, hydropolysulfides, or polysulfides having thio groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/14—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a synthesis process of diisoamyl sulfide, which comprises the steps of dissolving anhydrous sodium sulfide in hot water, adding absolute ethyl alcohol, heating and stirring, slowly dripping bromoisopentane when the mixture is subjected to reflux reaction, obtaining a reaction mixture upper layer which is crude diisoamyl sulfide, repeatedly washing the crude diisoamyl sulfide, and repeatedly carrying out reduced pressure distillation and purification to obtain the high-purity diisoamyl sulfide, wherein the whole production process has short flow, low labor intensity, less energy consumption, low production cost and short production period, the purity of the obtained diisoamyl sulfide can reach 99.5%, the yield is 80-85%, and the palladium extraction efficiency can be improved to more than 99.5%.
Description
Technical Field
The invention relates to the technical field of synthesis processes of novel palladium extractants, in particular to a synthesis process of diisoamyl sulfide.
Background
Diisoamyl sulfide is a common palladium extractant, and the synthesis process for producing the palladium extractant at home and abroad basically adopts bromoisopentane, ethanol and sodium sulfide are added for reflux reaction, precipitated oil is removed after the palladium extractant is cooled to room temperature, and then the residual reflux liquid is poured into sodium chloride aqueous solution with a certain concentration, and the precipitated oil is also separated and removed. The oil fractions were then combined, dried over anhydrous sodium sulfate, and distilled twice through a 36cm Hempel fractionating column packed with glass beads to give the noble metal extractant diisoamyl sulfide.
The original technology has the problems that: 1) The produced palladium extractant diisoamyl sulfide has unstable performance, poor quality and large odor, and can co-extract bivalent platinum, and the platinum-palladium extraction separation selectivity is not high, so that the direct yield of palladium is affected; 2) Copper chloride is added before diisoamyl sulfide extraction for deodorization, so that the diisoamyl sulfide can be used, is time-consuming and high in cost, is easy to crystallize, and brings difficulty to subsequent separation and purification; 3) The diisoamyl sulfide has small palladium extraction capacity, can not effectively improve the concentration of the palladium stock solution and can not improve the production efficiency; 4) The purity of the produced diisoamyl sulfide is not high, and the extraction rate is only 98%; 5) The direct yield of diisoamyl sulfide is low, only 59%; 6) The original process flow is long, more chemical reagents are needed, the overhaul rate of special 36cm Hempel fractionating column equipment is high, and the production cost is high.
Disclosure of Invention
The invention aims at solving the technical problems of low direct yield, high cost, high purification difficulty and low purity of the palladium extractant diisoamyl sulfide synthesis process, and provides a high-yield, high-purity and low-cost diisoamyl sulfide synthesis process.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
step one, dissolving: dissolving anhydrous sodium sulfide in hot water at 40-50 ℃ in a reaction kettle, adding absolute ethyl alcohol, heating the temperature in the reaction kettle to constant temperature of 74 ℃ and starting a stirring device; the mass ratio of the anhydrous sodium sulfide to the hot water to the anhydrous ethanol is 1.1:1.25:1;
step two, reflux: under the stirring condition of constant temperature of 74 ℃, when absolute ethyl alcohol in a reaction kettle starts to reflux, dropwise adding bromoisopentane into the mixed solution prepared in the step one, controlling the dropwise adding speed to be 1.0-1.1L/h, continuously heating and refluxing for reaction for 5-8 h after the dropwise adding is finished, and cooling to room temperature after the reaction is finished to obtain a mixture; the mass ratio of the adding amount of the bromoisopentane solution to the anhydrous sodium sulfide is 3:1; the mixture is in two phases, the upper layer is coarse diisoamyl sulfide accounting for 2/5 of the total volume, the lower layer is water-soluble sodium salt, mainly ethanol and sodium bromide solution accounting for 3/5 of the total volume, and the mixture can be recycled;
step three, filtering and washing: continuously washing the crude diisoamyl sulfide prepared in the step two with a sodium hydroxide solution with the mass percent concentration of 30% for 2 times, and then washing with hot water at the temperature of 40-50 ℃ until the PH value of the solution is equal to 7; the volume ratio of the crude diisoamyl sulfide to the sodium hydroxide solution to the hot water is 2:1:1;
step four, vacuum distillation and purification: adding the crude diisoamyl sulfide prepared in the step three into a reaction kettle, heating to 100 ℃, preserving heat for 0.5-1 h, and distilling unreacted alcohol and water vapor; then pumping into a vacuum pump to be vacuumized to 21.33-14.66KPa, heating to 118-122 ℃ and distilling under reduced pressure to remove unreacted bromoisopentane until no effluent liquid is recovered to normal pressure and replacing a receiving bottle; vacuumizing to 80KPa (15 mmHg), heating to 185-207 ℃ for secondary reduced pressure distillation, collecting distilled products, and performing reduced pressure distillation for 2 times according to the process to obtain diisoamyl sulfide;
the purity of the diisoamyl sulfide can reach 99.5% by adopting a gas chromatography analysis method, and the yield is 80-85%.
Preferably, the drop velocity of the bromoisopentane in the step II is less than or equal to the reflux velocity of the absolute ethanol.
The working principle of the invention is as follows: the normal pressure synthesis is to take ethanol as a catalyst, under the condition of heating, the bromoisopentane and sodium sulfide react chemically to generate diisoamyl sulfide, and phase separation is carried out according to the different densities of an oil phase and a water phase and the incompatibility; the purpose of adding sodium hydroxide is to wash and remove impurities, remove a small amount of acetic acid in ethanol, and wash with water to dissolve water-soluble impurities and sodium salt in the oil phase. If enough quicklime is added, acetic acid and calcium oxide react to generate calcium acetate, and the purpose of reduced pressure distillation is to separate the calcium acetate, the ethanol, the bromoisopentane and the diisoamyl sulfide by distillation under reduced pressure according to different air pressures and different boiling points of the water, the ethanol, the bromoisopentane and the diisoamyl sulfide.
The chemical reaction equation in the above steps is:
X＝Br
CH 3 COOH+NaOH＝CH 3 COONa+H 2 O。
compared with the prior art, the invention has the following advantages:
(1) The diisoamyl sulfide synthesis process adopts the steps of dissolution, reflux, filtering and washing, and reduced pressure distillation and purification, shortens the preparation flow of the diisoamyl sulfide, adopts the optimal feed liquid proportion and reasonable technical parameters, reduces excessive waste of raw materials, and enables the raw materials to fully and completely react.
(2) The diisoamyl thioether synthesis process adopts a multistage negative pressure absorption process to replace a 36cm Hempel fractionation method filled with glass beads, avoids a step of drying anhydrous sodium sulfate, reduces the preparation cost and reduces the energy consumption; the liquid in the multistage negative pressure absorption bottle is returned to the negative pressure distillation kettle for circulation, so that the direct yield of the diisoamyl sulfide product can be improved.
(3) The diisoamyl sulfide is prepared by adopting pure water to replace common water in the synthesis process of the diisoamyl sulfide, so that the highest purity of the product is ensured, and the performance is better.
Drawings
FIG. 1 is a flow chart of the synthesis process of diisoamyl sulfide of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
A synthesis process of diisoamyl sulfide, comprising the following steps:
step one, dissolving: 1.1kg of anhydrous sodium sulfide is dissolved in 1.25kg of hot water at 40 ℃ in a reaction kettle, 1kg of absolute ethyl alcohol is added, the temperature in the reaction kettle is heated to constant temperature of 74 ℃ and a stirring device is started;
step two, reflux: under the stirring condition of constant temperature of 74 ℃, when absolute ethyl alcohol in a reaction kettle starts to reflux, 3.3kg of isopentane bromide solution with the mass percent concentration of 99% is dripped into the mixed solution prepared in the step one, the dripping speed is controlled at 1.0L/h, the heating reflux reaction is continued for 5h after the dripping is finished, and 2500ml of mixture is obtained after the reaction is completed and cooled to room temperature; the mixture is in two phases, and the upper layer is 1000ml of crude diisoamyl sulfide aqueous solution; the lower layer is 1500ml of water-soluble sodium salt impurity, and the main components are ethanol and sodium bromide solution which can be recycled and reused;
step three, filtering and washing: continuously washing 1000mL of the crude diisoamyl sulfide aqueous solution prepared in the step two with 500mL of 30% sodium hydroxide solution for 2 times, and then continuously washing with 500mL of 40 ℃ hot water for 3 times until the pH value of the solution is equal to 7;
step four, vacuum distillation and purification: adding the crude diisoamyl sulfide prepared in the step three into a reaction kettle, heating to 100 ℃, preserving heat for 0.5h, and distilling unreacted alcohol and water vapor; then pumping into a vacuum pump to be vacuumized to 14.33KPa, heating to 120 ℃ and distilling under reduced pressure to remove unreacted bromoisopentane until no effluent liquid is discharged, recovering to normal pressure and replacing a receiving bottle; vacuumizing to 80KPa (15 mmHg), heating to 205 ℃ for secondary reduced pressure distillation, collecting distilled products, and performing reduced pressure distillation for 2 times according to the process to obtain 900ml of diisoamyl sulfide;
the purity of the diisoamyl sulfide is 99.5% by gas chromatography, the yield is 80%, and the palladium extraction rate is 99.5%.
Example 2
Step one, dissolving: 2.2kg of anhydrous sodium sulfide is dissolved in 2.5kg of hot water with the temperature of 50 ℃ in a reaction kettle, 2kg of absolute ethyl alcohol is added, the temperature in the reaction kettle is heated to the constant temperature of 74 ℃ and a stirring device is started;
step two, reflux: under the stirring condition of constant temperature of 74 ℃, when absolute ethyl alcohol in a reaction kettle starts to reflux, 6.6kg of isopentane bromide solution with the mass percent concentration of 99% is dripped into the mixed solution prepared in the step one, the dripping speed is controlled at 1.1L/h, the heating reflux reaction is continued for 8h after the dripping is finished, and the mixture is cooled to room temperature after the reaction is finished to obtain 5000ml of mixture; the mixture is in two phases, the upper layer is 2000ml of crude diisoamyl sulfide, the lower layer is 3000ml of water-soluble sodium salt, mainly ethanol and sodium bromide solution, and the mixture can be recycled;
step three, filtering and washing: continuously washing 2000ml of crude diisoamyl sulfide prepared in the second step with 1000ml of sodium hydroxide solution with the mass percent concentration of 30% for 2 times, and then continuously washing with 1000ml of hot water with the temperature of 50 ℃ for 3 times until the PH value of the solution is equal to 7;
step four, vacuum distillation and purification: adding 2000ml of crude diisoamyl sulfide prepared in the step three into a reaction kettle, heating to 100 ℃, preserving heat for 1h, and distilling unreacted alcohol and water vapor; then pumping into a vacuum pump to be vacuumized to 14.66KPa, heating to 122 ℃ and distilling under reduced pressure to remove unreacted bromoisopentane until no effluent liquid is discharged, recovering to normal pressure and replacing a receiving bottle; vacuumizing to 80KPa (15 mmHg), heating to 207 ℃ for secondary reduced pressure distillation, collecting distilled products, and performing reduced pressure distillation for 2 times according to the process to obtain 1800ml of diisoamyl sulfide;
the purity of the diisoamyl sulfide can reach 99.5% by adopting a gas chromatography analysis, the yield is 85%, and the palladium extraction rate is 99.5%.
Example 3
A synthesis process of diisoamyl sulfide, comprising the following steps:
step one, dissolving: dissolving 3.3kg of anhydrous sodium sulfide in 3.75kg of hot water at 45 ℃ in a reaction kettle, adding 3kg of absolute ethyl alcohol, heating the temperature in the reaction kettle to constant temperature of 74 ℃ and starting a stirring device; the mass ratio of the anhydrous sodium sulfide to the hot water to the anhydrous ethanol is 1.1:1.25:1;
step two, reflux: under the stirring condition of constant temperature of 74 ℃, when absolute ethyl alcohol in a reaction kettle starts to reflux, 9.9kg of the isopentane bromide solution with the mass percent concentration of 99% is dripped into the mixed solution prepared in the step one, the dripping speed is controlled at 1.05L/h, the heating reflux reaction is continued for 6h after the dripping is finished, and 7500ml of mixture is obtained after the reaction is finished and cooled to room temperature; the mixture is in two phases, the upper layer is 3000ml of crude diisoamyl sulfide, the lower layer is 4500ml of water-soluble sodium salt, and the mixture is mainly ethanol and sodium bromide solution, and can be recycled;
step three, filtering and washing: continuously washing 3000ml of crude diisoamyl sulfide prepared in the second step with 1500ml of sodium hydroxide solution with the mass percent concentration of 30% for 2 times, and then continuously washing with 1500ml of hot water with the temperature of 45 ℃ for 3 times until the PH value of the solution is equal to 7;
step four, vacuum distillation and purification: adding 3000ml of crude diisoamyl sulfide prepared in the step three into a reaction kettle, heating to 100 ℃, preserving heat for 0.8h, and distilling unreacted alcohol and water vapor; then pumping into a vacuum pump to be vacuumized to 14.5KPa, heating to 120 ℃ and distilling under reduced pressure to remove unreacted bromoisopentane until no effluent liquid is discharged, recovering to normal pressure and replacing a receiving bottle; vacuumizing to 80KPa (15 mmHg), heating to 206 ℃, performing secondary reduced pressure distillation, collecting distilled products, and performing reduced pressure distillation for 2 times according to the process to obtain 2250mL of diisoamyl sulfide;
the purity of the diisoamyl sulfide can reach 99.5% by adopting a gas chromatography analysis, the yield is 83%, and the palladium extraction rate is 99.6%.
The product yields and analytical results are shown in Table 1.
TABLE 1 product yields and analytical results Table
| Numbering device | Yield (%) | Purity (%) | Palladium extraction yield (%) |
| Example 1 | 80 | 99.5 | 99.5 |
| Example 2 | 85 | 99.5 | 99.5 |
| Example 3 | 83 | 99.5 | 99.6 |
It can be concluded from the data in table 1 that examples 1-3 are the synthesis processes for diisoamyl sulfide provided by the present invention, which can obtain diisoamyl sulfide with high yield, high purity and high palladium extraction rate. The method is successfully applied to a noble metal palladium extraction production line of a certain company, the method is adopted to ensure that the high-purity diisoamyl sulfide is self-produced, 3 tons of high-purity diisoamyl sulfide produced each year is applied to production, the palladium extraction performance is good, the concentration of platinum and palladium in the palladium extraction stock solution is improved to more than 28g/L from 16g/L, and the production efficiency is improved by 1 time; meanwhile, the performance of the co-extraction of bivalent platinum is reduced, platinum and palladium are effectively separated, and the efficiency of extracting palladium can be improved to more than 99.5%.
Claims (2)
1. A synthesis process of diisoamyl sulfide is characterized in that: the method comprises the following steps:
step one, dissolving: dissolving anhydrous sodium sulfide in hot water at 40-50 ℃ in a reaction kettle, adding absolute ethyl alcohol, heating the temperature in the reaction kettle to constant temperature of 74 ℃ and starting a stirring device; the mass ratio of the anhydrous sodium sulfide to the hot water to the anhydrous ethanol is 1.1:1.25:1;
step two, reflux: under the stirring condition of constant temperature of 74 ℃, when absolute ethyl alcohol in a reaction kettle starts to reflux, dropwise adding a brominated isopentane solution with the mass percent concentration of 99% into the mixed solution prepared in the step one, controlling the dropwise adding speed to be 1.0-1.1L/h, continuing to heat and reflux for 5-8 h after the dropwise adding, and cooling to room temperature after the reaction is finished to obtain a mixture; the mass ratio of the adding amount of the bromoisopentane solution to the anhydrous sodium sulfide is 3:1; the mixture is in two phases, the upper layer is coarse diisoamyl sulfide accounting for 2/5 of the total volume, the lower layer is water-soluble sodium salt, mainly ethanol and sodium bromide solution accounting for 3/5 of the total volume, and the mixture can be recycled;
step three, filtering and washing: continuously washing the crude diisoamyl sulfide prepared in the step two with a sodium hydroxide solution with the mass percent concentration of 30% for 2 times, and then washing with hot water at the temperature of 40-50 ℃ until the PH value of the solution is equal to 7; the volume ratio of the crude diisoamyl sulfide to the sodium hydroxide solution to the hot water is 2:1:1;
step four, vacuum distillation and purification: adding the crude diisoamyl sulfide prepared in the step three into a reaction kettle, heating to 100 ℃, preserving heat for 0.5-1 h, and distilling unreacted alcohol and water vapor; then pumping into a vacuum pump to be vacuumized to 21.33-14.66KPa, heating to 118-122 ℃ and distilling under reduced pressure to remove unreacted bromoisopentane until no effluent liquid is recovered to normal pressure and replacing a receiving bottle; vacuumizing to 80KPa (15 mmHg), heating to 185-207 ℃ for secondary reduced pressure distillation, collecting distilled products, and performing reduced pressure distillation for 2 times according to the process to obtain diisoamyl sulfide;
the purity of the diisoamyl sulfide can reach 99.5% by adopting a gas chromatography analysis method, and the yield is 80-85%.
2. The process according to claim 1, wherein the drop velocity of bromoisopentane in step two is less than or equal to the reflux velocity of absolute ethanol.
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