CN114409619A - Production method of difurfuryl sulfide - Google Patents
Production method of difurfuryl sulfide Download PDFInfo
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- CN114409619A CN114409619A CN202210077281.5A CN202210077281A CN114409619A CN 114409619 A CN114409619 A CN 114409619A CN 202210077281 A CN202210077281 A CN 202210077281A CN 114409619 A CN114409619 A CN 114409619A
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- UYLKDZXJEKFFHJ-UHFFFAOYSA-N 2-(furan-2-ylmethylsulfanylmethyl)furan Chemical compound C=1C=COC=1CSCC1=CC=CO1 UYLKDZXJEKFFHJ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 claims abstract description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- GANBJDIOIDQSGI-UHFFFAOYSA-N 2-(chloromethyl)furan Chemical compound ClCC1=CC=CO1 GANBJDIOIDQSGI-UHFFFAOYSA-N 0.000 claims abstract description 20
- ZFFTZDQKIXPDAF-UHFFFAOYSA-N 2-Furanmethanethiol Chemical compound SCC1=CC=CO1 ZFFTZDQKIXPDAF-UHFFFAOYSA-N 0.000 claims abstract description 11
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims abstract description 9
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract 3
- 238000001816 cooling Methods 0.000 claims description 40
- 239000012074 organic phase Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 24
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 11
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- 239000012043 crude product Substances 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000008346 aqueous phase Substances 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 230000003472 neutralizing effect Effects 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 5
- OFTKFKYVSBNYEC-UHFFFAOYSA-N 2-furoyl chloride Chemical compound ClC(=O)C1=CC=CO1 OFTKFKYVSBNYEC-UHFFFAOYSA-N 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000006467 substitution reaction Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000011112 process operation Methods 0.000 abstract 1
- 239000007858 starting material Substances 0.000 abstract 1
- 150000003568 thioethers Chemical class 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 244000299461 Theobroma cacao Species 0.000 description 2
- 235000016213 coffee Nutrition 0.000 description 2
- 235000013353 coffee beverage Nutrition 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 240000007154 Coffea arabica Species 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 235000009470 Theobroma cacao Nutrition 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000013330 chicken meat Nutrition 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 235000019219 chocolate Nutrition 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 230000019086 sulfide ion homeostasis Effects 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
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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 production method of difurfuryl sulfide, which takes furfuryl alcohol as a starting material and prepares the difurfuryl sulfide through three steps of reaction operations, and furfuryl chloride is prepared by furfuryl alcohol and phosphorus trichloride; then sodium hydroxide, water and furfuryl mercaptan are used to prepare furfuryl sodium mercaptan, and furfuryl chloride and furfuryl mercaptan are used to prepare difurfuryl thioether through substitution and addition. The invention has the beneficial effects that: the method has the advantages of safety, environmental protection, simple and easy process operation, high finished product content, easily obtained raw materials, low production cost, suitability for large-scale production and wide production prospect.
Description
Technical Field
The invention relates to the technical field of food additive production, in particular to a production method of difurfuryl sulfide.
Background
The difurfuryl sulfide is a sulfur-containing spice, has nut fragrance and roasted coffee fragrance, and is an edible essence which can be used for preparing coffee, cocoa, chocolate, delicious food, chicken, beef and other flavors.
Difurfuryl sulfide of the formula C10H10O2S, the structural formula is shown as follows.
At present, few research reports on the synthesis of difurfuryl sulfide exist, and the following problems exist in the existing difurfuryl sulfide production process: the chlorination reaction operation is carried out under normal pressure, a large amount of ether escapes in the reaction process, which wastes raw materials and causes environmental pollution, and after the condensation reaction is finished, all the ether in the reaction system is washed by water, which wastes raw materials and increases the operation difficulty.
Disclosure of Invention
The present invention aims at providing a production method of difurfuryl sulfide to solve the technical problems.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for producing difurfuryl sulfide, comprising the steps of:
step 1) preparing furfuryl chloride;
(1) taking one three-neck flask, installing a stirrer, a thermometer and a constant pressure dropping funnel, and placing the lower part of the three-neck flask in an ice salt bath barrel for cooling;
(2) adding furfuryl alcohol into a three-neck flask, and stirring after adding;
(3) slowly cooling to below-5 ℃ under stirring;
(4) controlling the temperature to be 0-10 ℃, and beginning to dropwise add phosphorus trichloride;
(5) after dripping, keeping the temperature for reaction for 1 hour;
(6) cooling to below 30 deg.c and discharging the base liquid to obtain coarse furfuryl chloride product.
Step 2) preparing sodium furfuryl mercaptide;
(1) taking one three-neck flask, installing a stirrer, a thermometer and a constant pressure dropping funnel, and placing the lower part of the three-neck flask in a water bath barrel for cooling;
(2) adding water and sodium hydroxide into a three-neck flask, stirring and dissolving after adding, simultaneously cooling to 40 ℃, beginning to dropwise add furfuryl mercaptan, controlling the temperature to be 40-50 ℃, dropwise adding, controlling the temperature to be 40-50 ℃ after dropwise adding, and carrying out heat preservation reaction for 2 hours for later use;
step 3) preparing difurfuryl sulfide;
(1) cooling the furfuryl sodium mercaptide solution to below 10 ℃ by using ice water;
(2) controlling the temperature to be 10-20 ℃, and beginning to dropwise add furfuryl chloride;
(3) controlling the temperature to be between 10 and 20 ℃ after dripping, and keeping the temperature to react for 1 hour;
(4) introducing steam, heating to reflux, and carrying out reflux reaction for 2 hours;
(5) cooling to room temperature, neutralizing the reaction solution with a 10% sodium carbonate solution until the pH is = 7-8, standing and layering, wherein an upper organic phase and a lower aqueous phase are obtained;
(6) adding water to wash the organic phase, stirring for 30 minutes, standing for layering, removing an upper organic phase and a lower water phase, and taking the organic phase as a crude product;
(7) and (3) carrying out reduced pressure rectification, and collecting the fraction at 135-143 ℃/14mmHg to obtain a difurfuryl sulfide finished product.
As a further scheme of the invention, the mass ratio of the furfuryl alcohol and the phosphorus trichloride in the step 1) is 3: 1.1 to 2.5.
As a further scheme of the invention, the mass ratio of the furfuryl mercaptan to the sodium hydroxide in the step 2) is 1: 1.0 to 2.5.
As a further scheme of the invention, the mass ratio of the sodium furfurylthiol to the furoyl chloride in the step 3) is 1: 1.2 to 2.5.
The reaction equation is as follows:
the invention has the beneficial effects that: 1) the reaction realizes the operation of replacing ether with water, reduces the processing difficulty of the solvent, reduces the production cost, simplifies the operation steps, and is environment-friendly and safe;
2) the product only washes the organic phase in the washing process, and no organic solvent is involved, so that the use amount of water is reduced, the generation amount of wastewater is reduced, and the wastewater treatment cost is greatly reduced.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
1) Synthesizing furfuryl chloride;
(1) taking one 1L three-neck flask, installing a stirrer, a thermometer and a constant pressure dropping funnel, and placing the lower part of the three-neck flask in an ice salt bath barrel for cooling;
(2) adding 180g of furfuryl alcohol into a three-neck flask, and stirring after adding;
(3) slowly cooling to below-5 ℃ under stirring;
(4) controlling the temperature to be 0-10 ℃, and beginning to dropwise add 84.8g of phosphorus trichloride;
(5) after dripping, keeping the temperature for reaction for 1 hour;
(6) cooling to below 30 deg.C, and discharging the base solution to obtain crude furfuryl chloride product 256.2g with content of 85.2%.
2) Synthesizing sodium furfurylthionolate;
(1) taking one 2L three-neck flask, installing a stirrer, a thermometer and a constant pressure dropping funnel, and placing the lower part of the three-neck flask in a water bath barrel for cooling;
(2) adding 420g of water and 35g of sodium hydroxide into a three-neck flask, stirring and dissolving after adding, simultaneously cooling to 40 ℃, beginning to dropwise add 86g of furfuryl mercaptan, controlling the temperature to be 40-50 ℃, dropwise adding, controlling the temperature to be 40-50 ℃, preserving the temperature and reacting for 2 hours after completing dropwise adding, and standing for later use.
3) Synthesizing difurfuryl sulfide;
(1) cooling the furfuryl sodium mercaptide solution to below 10 ℃ by using ice water;
(2) controlling the temperature to be 10-20 ℃, and beginning to dropwise add furfuryl chloride;
(3) controlling the temperature to be between 10 and 20 ℃ after dripping, and keeping the temperature to react for 1 hour;
(4) introducing steam, heating to reflux, and carrying out reflux reaction for 2 hours;
(5) cooling to room temperature, neutralizing the reaction solution with a 10% sodium carbonate solution until the pH is = 7-8, standing for layering, removing an upper organic phase and a lower aqueous phase;
(6) adding water to wash the organic phase, stirring for 30 minutes, standing for layering, removing an upper organic phase and a lower water phase, wherein the organic phase is 256.5g of crude product and the content is 84.6%;
(7) and (3) carrying out reduced pressure rectification, and collecting 135-143 ℃/14mmHg fractions which are 197g of difurfuryl sulfide finished products with the content of 99.2%.
Example 2
1) Synthesizing furfuryl chloride;
(1) taking one 2L three-neck flask, installing a stirrer, a thermometer and a constant pressure dropping funnel, and placing the lower part of the three-neck flask in an ice salt bath barrel for cooling;
(2) adding 360g of furfuryl alcohol into a three-neck flask, and stirring after adding;
(3) slowly cooling to below-5 ℃ under stirring;
(4) controlling the temperature to be 0-10 ℃, and beginning to dropwise add 170g of phosphorus trichloride;
(5) after dripping, keeping the temperature for reaction for 1 hour;
(6) cooling to below 30 deg.C, and discharging the base solution to obtain crude furfuryl chloride product 500g with content of 85.2%.
2) Synthesizing sodium furfurylthionolate;
(1) taking one 5L three-neck flask, installing a stirrer, a thermometer and a constant pressure dropping funnel, and placing the lower part of the three-neck flask in a water bath barrel for cooling;
(2) 840g of water and 70g of sodium hydroxide are added into a three-neck flask, stirring and dissolving are carried out after the addition, 172g of furfuryl mercaptan is dripped when the temperature is reduced to 40 ℃, the temperature is controlled to be 40-50 ℃, and the temperature is controlled to be 40-50 ℃ after the dripping, and the reaction is carried out for 2 hours for standby application.
3) Synthesizing difurfuryl sulfide;
(1) cooling the furfuryl sodium mercaptide solution to below 10 ℃ by using ice water;
(2) controlling the temperature to be 10-20 ℃, and beginning to dropwise add furfuryl chloride;
(3) controlling the temperature to be between 10 and 20 ℃ after dripping, and keeping the temperature to react for 1 hour;
(4) introducing steam, heating to reflux, and carrying out reflux reaction for 2 hours;
(5) cooling to room temperature, neutralizing the reaction solution with a 10% sodium carbonate solution until the pH is = 7-8, standing for layering, removing an upper organic phase and a lower aqueous phase;
(6) adding water to wash the organic phase, stirring for 30 minutes, standing for layering, removing an upper organic phase and a lower water phase, wherein the organic phase is 510g of crude product and the content is 84.6%;
(7) reduced pressure rectification is carried out, and the distillate with 135-143 ℃/14mmHg is collected to be 400g of difurfuryl sulfide finished product with the content of 99.2 percent.
Example 3
1) Synthesizing furfuryl chloride;
(1) taking one 5L three-neck flask, installing a stirrer, a thermometer and a constant pressure dropping funnel, and placing the lower part of the three-neck flask in an ice salt bath barrel for cooling;
(2) adding 720g of furfuryl alcohol into a three-neck flask, and stirring after adding;
(3) slowly cooling to below-5 ℃ under stirring;
(4) controlling the temperature to be 0-10 ℃, and beginning to dropwise add 340g of phosphorus trichloride;
(5) after dripping, keeping the temperature for reaction for 1 hour;
(6) cooling to below 30 deg.C, and discharging the base solution to obtain crude furfuryl chloride product 1000g with content of 85.2%.
2) Synthesizing sodium furfurylthionolate;
(1) taking one 10L three-neck flask, installing a stirrer, a thermometer and a constant pressure dropping funnel, and placing the lower part of the three-neck flask in a water bath barrel for cooling;
(2) adding 1700g of water and 140g of sodium hydroxide into a three-neck flask, stirring and dissolving after adding, simultaneously cooling to 40 ℃, beginning to dropwise add 340g of furfuryl mercaptan, controlling the temperature to be 40-50 ℃, dropwise adding, controlling the temperature to be 40-50 ℃, keeping the temperature and reacting for 2 hours after completing dropwise adding, and standing for later use.
3) Synthesizing difurfuryl sulfide;
(1) cooling the furfuryl sodium mercaptide solution to below 10 ℃ by using ice water;
(2) controlling the temperature to be 10-20 ℃, and beginning to dropwise add furfuryl chloride;
(3) controlling the temperature to be between 10 and 20 ℃ after dripping, and keeping the temperature to react for 1 hour;
(4) ventilating, heating to reflux, and reacting for 2 hours under reflux;
(5) cooling to room temperature, neutralizing the reaction solution with a 10% sodium carbonate solution until the pH is = 7-8, standing for layering, removing an upper organic phase and a lower aqueous phase;
(6) adding water to wash the organic phase, stirring for 30 minutes, standing for layering, removing an upper organic phase and a lower water phase, wherein the organic phase is 1050g of crude product and the content is 84.6%;
(7) reduced pressure rectification is carried out, and the distillate with 135-143 ℃/14mmHg is collected to be 800g of difurfuryl sulfide finished product with the content of 99.2 percent.
Example 4
1) Synthesizing furfuryl chloride;
(1) taking one 10L three-neck flask, installing a stirrer, a thermometer and a constant pressure dropping funnel, and placing the lower part of the three-neck flask in an ice salt bath barrel for cooling;
(2) 1400g of furfuryl alcohol is added into a three-neck flask, and stirring is carried out after the addition is finished;
(3) slowly cooling to below-5 ℃ under stirring;
(4) controlling the temperature to be 0-10 ℃, and starting to dropwise add 680g of phosphorus trichloride;
(5) after dripping, keeping the temperature for reaction for 1 hour;
(6) cooling to below 30 deg.C, and discharging the base solution to obtain furfuryl chloride crude product 2000g with content of 85.2%.
2) Synthesizing sodium furfurylthionolate;
(1) taking one 20L three-neck flask, installing a stirrer, a thermometer and a constant pressure dropping funnel, and placing the lower part of the three-neck flask in a water bath barrel for cooling;
(2) 3500g of water and 280g of sodium hydroxide are added into a three-neck flask, stirring and dissolving are carried out after the addition, 680g of furfuryl mercaptan is dripped when the temperature is reduced to 40 ℃, the temperature is controlled to be 40-50 ℃, and the temperature is controlled to be 40-50 ℃ after the dripping, and the reaction is carried out for 2 hours for standby application.
3) Synthesizing difurfuryl sulfide;
(1) cooling the furfuryl sodium mercaptide solution to below 10 ℃ by using ice water;
(2) controlling the temperature to be 10-20 ℃, and beginning to dropwise add furfuryl chloride;
(3) controlling the temperature to be between 10 and 20 ℃ after dripping, and keeping the temperature to react for 1 hour;
(4) ventilating, heating to reflux, and reacting for 2 hours under reflux;
(5) cooling to room temperature, neutralizing the reaction solution with a 10% sodium carbonate solution until the pH is = 7-8, standing for layering, removing an upper organic phase and a lower aqueous phase;
(6) adding water to wash the organic phase, stirring for 30 minutes, standing for layering, removing an upper organic phase and a lower aqueous phase, wherein the organic phase is 2100g of crude product and the content is 84.6%;
(7) reduced pressure rectification is carried out, and the distillate with the temperature of 135-143 ℃/14mmHg is collected to be 1600g of difurfuryl sulfide finished product with the content of 99.2 percent.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A production method of difurfuryl sulfide is characterized by comprising the following steps:
step 1) preparing furfuryl chloride;
(1) taking one three-neck flask, installing a stirrer, a thermometer and a constant pressure dropping funnel, and placing the lower part of the three-neck flask in an ice salt bath barrel for cooling;
(2) adding furfuryl alcohol into a three-neck flask, and stirring after adding;
(3) slowly cooling to below-5 ℃ under stirring;
(4) controlling the temperature to be 0-10 ℃, and beginning to dropwise add phosphorus trichloride;
(5) after dripping, keeping the temperature for reaction for 1 hour;
(6) cooling to below 30 ℃, and discharging the base solution for later use to obtain a furfuryl chloride crude product;
step 2) preparing sodium furfuryl mercaptide;
(1) taking one three-neck flask, installing a stirrer, a thermometer and a constant pressure dropping funnel, and placing the lower part of the three-neck flask in a water bath barrel for cooling;
(2) adding water and sodium hydroxide into a three-neck flask, stirring and dissolving after adding, simultaneously cooling to 40 ℃, beginning to dropwise add furfuryl mercaptan, controlling the temperature to be 40-50 ℃, dropwise adding, controlling the temperature to be 40-50 ℃ after dropwise adding, and carrying out heat preservation reaction for 2 hours for later use;
step 3) preparing difurfuryl sulfide;
(1) cooling the furfuryl sodium mercaptide solution to below 10 ℃ by using ice water;
(2) controlling the temperature to be 10-20 ℃, and beginning to dropwise add furfuryl chloride;
(3) controlling the temperature to be between 10 and 20 ℃ after dripping, and keeping the temperature to react for 1 hour;
(4) introducing steam, heating to reflux, and carrying out reflux reaction for 2 hours;
(5) cooling to room temperature, neutralizing the reaction solution with a 10% sodium carbonate solution until the pH is = 7-8, standing and layering, wherein an upper organic phase and a lower aqueous phase are obtained;
(6) adding water to wash the organic phase, stirring for 30 minutes, standing for layering, removing an upper organic phase and a lower water phase, and taking the organic phase as a crude product;
(7) and (3) carrying out reduced pressure rectification, and collecting the fraction at 135-143 ℃/14mmHg to obtain a difurfuryl sulfide finished product.
2. The process for producing difurfuryl sulfide according to claim 1, wherein the mass ratio of furfuryl alcohol and phosphorus trichloride in step 1) is 3: 1.1 to 2.5.
3. The process for producing difurfuryl sulfide according to claim 1, wherein the mass ratio of furfuryl mercaptan to sodium hydroxide in the step 2) is 1: 1.0 to 2.5.
4. The method for producing difurfuryl sulfide according to claim 1, wherein the mass ratio of the sodium furfuryl sulfate to the furoyl chloride in the step 3) is 1: 1.2 to 2.5.
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