CN112457223B - Degassing process for producing sodium hexadecylsulfonate - Google Patents
Degassing process for producing sodium hexadecylsulfonate Download PDFInfo
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- CN112457223B CN112457223B CN202011330080.9A CN202011330080A CN112457223B CN 112457223 B CN112457223 B CN 112457223B CN 202011330080 A CN202011330080 A CN 202011330080A CN 112457223 B CN112457223 B CN 112457223B
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- degassing tank
- pipe
- degassing
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- sulfonyl chloride
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- 238000007872 degassing Methods 0.000 title claims abstract description 127
- PNGBYKXZVCIZRN-UHFFFAOYSA-M sodium;hexadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCS([O-])(=O)=O PNGBYKXZVCIZRN-UHFFFAOYSA-M 0.000 title claims abstract description 24
- 125000004390 alkyl sulfonyl group Chemical group 0.000 claims abstract description 44
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000007789 gas Substances 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 23
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000460 chlorine Substances 0.000 claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 10
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 238000004321 preservation Methods 0.000 claims abstract description 10
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 9
- 239000000295 fuel oil Substances 0.000 claims abstract description 8
- OSVXSBDYLRYLIG-UHFFFAOYSA-N chlorine dioxide Inorganic materials O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000019398 chlorine dioxide Nutrition 0.000 claims abstract description 7
- 230000007246 mechanism Effects 0.000 claims description 37
- 238000003756 stirring Methods 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 15
- 238000007599 discharging Methods 0.000 claims description 12
- 238000005507 spraying Methods 0.000 claims description 10
- 239000006227 byproduct Substances 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 238000005286 illumination Methods 0.000 claims description 5
- 210000000621 bronchi Anatomy 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000004891 communication Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 238000002386 leaching Methods 0.000 abstract description 2
- 238000010907 mechanical stirring Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 23
- 238000002347 injection Methods 0.000 description 14
- 239000007924 injection Substances 0.000 description 14
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 8
- YOSVFFVBSPQTTP-UHFFFAOYSA-N hexadecane-1-sulfonyl chloride Chemical compound CCCCCCCCCCCCCCCCS(Cl)(=O)=O YOSVFFVBSPQTTP-UHFFFAOYSA-N 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 238000000605 extraction Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- -1 sodium alkyl sulfonate Chemical class 0.000 description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 description 4
- UJGIYHXRNBCGRE-UHFFFAOYSA-N C(CCCCCCCCCCCCCCC)[Na] Chemical compound C(CCCCCCCCCCCCCCC)[Na] UJGIYHXRNBCGRE-UHFFFAOYSA-N 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000007127 saponification reaction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000005694 sulfonylation reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/10—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfur dioxide and halogen or by reaction with sulfuryl halides
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Degasification And Air Bubble Elimination (AREA)
Abstract
The invention discloses a degassing process for producing sodium hexadecyl sulfonate, which comprises the following steps of: step one, adding heavy oil into a reaction kettle, and introducing a mixed gas of chlorine and sulfur dioxide into the reaction kettle to obtain an alkyl sulfonyl chloride mixture; secondly, putting the mixture of alkyl sulfonyl chloride into a degassing device through a feeding pipe to obtain purified alkyl sulfonyl chloride; thirdly, adding the purified alkyl sulfonyl chloride into a reaction tank filled with a sodium hydroxide solution, and reacting for 1-2h to obtain a mixed solution A; and step four, purifying and separating the mixed solution A to obtain the sodium hexadecyl sulfonate, removing chlorine, sulfur dioxide and hydrogen chloride gas in the mixture of the alkyl sulfonyl chlorides by a method combining mechanical stirring and hot gas leaching, wherein the degassing device has the characteristics of heat preservation, convenience in blanking, safety in use and the like.
Description
Technical Field
The invention belongs to the technical field of sodium hexadecyl sulfonate production, and particularly relates to a degassing process for producing sodium hexadecyl sulfonate.
Background
The sodium hexadecyl sulfonate is an anionic surfactant with good water solubility, has good wetting, emulsifying, dispersing, foaming and decontamination capabilities in hard water, has good biodegradability and small stimulation to human bodies, and is used for industrial detergents, civil liquid detergents, textile industry cleaning agents, dyeing assistants and flotation agents for mineral separation.
Sodium hexadecyl sulfonate product is water white turbid liquid and is at 20 DEG CDensity of 1.055g/cm3The viscosity is 0.02Pa.s, the flash point is more than 100 ℃, the heavy oil generally undergoes sulfonylation reaction under the condition of sulfur dioxide and chlorine gas in the industrial production process to obtain hexadecyl sulfonyl chloride, the hexadecyl sulfonyl chloride is degassed to remove the chlorine gas, the sulfur dioxide and the byproduct hydrogen chloride gas which are not completely reacted in the liquid, then the hexadecyl sulfonyl chloride reacts with the sodium hydroxide solution for saponification reaction, and the finished product of the hexadecyl sodium sulfonate is obtained after separation.
In the prior art, the degassing process of hexadecyl sulfonyl chloride is complicated and incomplete in degassing, so that the purity of the hexadecyl sulfonyl chloride is low, the impurity content in a finished product of the hexadecyl sodium sulfonate is high, the yield is low, and chlorine, sulfur dioxide and a byproduct hydrogen chloride gas which are not completely reacted in liquid can cause environmental pollution and seriously harm human health. Therefore, the improvement of the degassing process for efficiently, thoroughly and comprehensively producing the sodium hexadecyl sulfonate is the technical problem to be solved at present.
Disclosure of Invention
The invention aims to provide a degassing process for producing sodium hexadecyl sulfonate.
The technical problems to be solved by the invention are as follows:
in the prior art, the degassing process of the hexadecyl sulfonyl chloride is complicated and incomplete in degassing, so that the purity of the hexadecyl sulfonyl chloride is low, the impurity content in a finished product of the hexadecyl sodium sulfonate is high, the yield is low, and the chlorine, the sulfur dioxide and a byproduct hydrogen chloride gas which are not completely reacted in the liquid can cause environmental pollution and harm human health in serious cases.
The purpose of the invention can be realized by the following technical scheme:
a degassing process for the production of sodium hexadecylsulfonate, comprising the steps of:
step one, adding heavy oil into a reaction kettle, introducing mixed gas consisting of chlorine and sulfur dioxide in a volume ratio of 1:2 into the reaction kettle under the illumination of ultraviolet rays, controlling the temperature in the reaction kettle to be 33 +/-2 ℃, and reacting for 3-5 hours under the condition of a rotation speed of 100 plus-one materials of 200r/min to obtain an alkyl sulfonyl chloride mixture;
secondly, putting the alkyl sulfonyl chloride mixture into a degassing device from a feeding pipe, removing chlorine, sulfur dioxide and a byproduct hydrogen chloride gas in the alkyl sulfonyl chloride mixture through the degassing device to obtain impurity-removed alkyl sulfonyl chloride liquid, and discharging the liquid out of the degassing device through a discharging pipe to obtain purified alkyl sulfonyl chloride;
thirdly, adding purified alkyl sulfonyl chloride into a reaction tank filled with 35% sodium hydroxide solution by mass fraction, keeping the temperature of the reaction tank at 95-100 ℃, and reacting for 1-2h under the condition of the rotation speed of 200-;
and fourthly, adding the mixed solution A into a heat preservation cylinder, preserving the heat for 4 hours at the temperature of 105-plus-110 ℃, separating a lower water phase B, adding the lower water phase B into the heat preservation cylinder again, preserving the heat for 8 hours at the temperature of 105-plus-110 ℃, separating a lower water phase C, adding a sodium bicarbonate solution with the mass fraction of 20% into the lower water phase C, and adjusting the pH value to 7-8 to obtain the sodium hexadecylsulfonate.
In the second step, the degassing device comprises a first supporting plate, a degassing tank and an auxiliary blanking mechanism, wherein the first supporting plate is a rectangular plate horizontally and transversely placed, four corners of the lower end of the first supporting plate are fixedly provided with connecting pieces, each connecting piece is movably connected with a universal wheel, the degassing tank is fixedly arranged above the first supporting plate, the auxiliary blanking mechanism is positioned on one side of the degassing tank and is supported and fixed by a second supporting plate, and one end of the second supporting plate is fixedly welded on the surface of one side of the degassing tank;
the upper end central point of degassing tank puts the fixed inlet pipe that is provided with, the inlet pipe passes degassing tank's upper wall and extends to degassing tank's inside, fixed mounting has the feed valve on the inlet pipe, the inlet pipe is the plastic hose, one side of inlet pipe is fixed and is provided with the exhaust tube, the one end of exhaust tube passes degassing tank's upper wall and extends to degassing tank's inside, the last fixed exhaust valve that is provided with of exhaust tube, the bottom mounting of exhaust tube has the active carbon adsorption plate, degassing tank's lower extreme central point is fixed and is provided with the discharge tube, the discharge tube passes first backup pad and extends to the lower extreme of first backup pad, the last fixed mounting of discharge tube has the discharge valve, degassing tank divide into two-layer inside and outside, degassing tank's inlayer bottom structure is circular-arc, be provided with the heating chamber between degassing tank's the inlayer, honeycomb duct one end passes degassing tank's outer wall and extends to in the heating chamber, fixed mounting has the control valve on the honeycomb duct, hot oil or hot water is injected into the guide pipe, enters a heating cavity of the degassing tank and provides heating conditions of constant-temperature water bath or constant-temperature oil bath for the degassing tank;
a third supporting plate is fixedly installed on one side of the outer wall of the degassing tank, a first motor is fixedly arranged on the third supporting plate, the output end of the first motor is fixedly connected with a stirring shaft through a coupler, one end of the stirring shaft penetrates through the heating cavity and extends into the degassing tank, a first bearing sleeve is fixedly sleeved on the stirring shaft and is in sealed connection with the inner wall and the outer wall of the degassing tank, a plurality of spiral stirring blades are fixedly connected on the stirring shaft, a first belt pulley is sleeved on one side, close to the first motor, of the stirring shaft, a second belt pulley is arranged above the first belt pulley, the first belt pulley is connected with the second belt pulley through a belt, the second belt pulley is sleeved on a threaded rod, one end of the threaded rod penetrates through the heating cavity and extends into the degassing tank, a second bearing sleeve is sleeved on one end, close to the second belt pulley, and is in sealed connection with the inner wall and the outer wall of the degassing tank, one end of the threaded rod, which is far away from the second belt pulley, is rotatably arranged in a third bearing sleeve, the third bearing sleeve is welded on the inner wall of the degassing tank, reverse threads which extend from the middle to the two ends are arranged on the threaded rod, two material spraying mechanisms are sleeved on the threaded rod in a threaded manner, each material spraying mechanism comprises a branch pipe and a spray head, the branch pipes are fixedly connected and communicated with the spray heads, movable blocks are fixedly sleeved on the branch pipes, the movable blocks are sleeved on the threaded rod, threads matched with the threaded rods are arranged in the movable blocks, the upper ends of the branch pipes are fixedly connected and communicated with material distributing pipes, and the middle parts of the material distributing pipes are fixedly connected and communicated with the feeding pipes;
a filter screen is fixedly arranged below the material spraying mechanism and supported and fixed by a circular table which is fixedly arranged on the inner wall of the degassing tank;
an air injection mechanism is fixedly arranged below the stirring shaft, the air injection mechanism comprises a branch air pipe, the branch air pipe is fixedly arranged at the upper end of an air injection head and is communicated with the air injection head, the lower end of the air injection head is fixedly connected and communicated with a connecting pipe, one end, far away from the air injection head, of the connecting pipe is fixedly connected and communicated with an air delivery pipe, one end, far away from the air injection head, of the air delivery pipe penetrates through the inner wall and the outer wall of the degassing tank to extend to the outside of the degassing tank and is communicated with an air storage tank, and a valve is fixedly arranged on the air delivery pipe;
the fixed second motor that is provided with in the second backup pad, the output of second motor passes through shaft coupling and lead screw fixed connection, the box outer wall that supplementary unloading mechanism was passed to the one end of lead screw and the middle part threaded connection of slide bar, the spout has been seted up to the lower extreme on the box of supplementary unloading mechanism, the upper and lower both ends fixedly connected with slider of slide bar, one side of slide bar is through two connecting rods and piston head fixed connection, the size of piston head and the box looks adaptation of supplementary unloading mechanism, the rectangle passageway is seted up to the one end of keeping away from the second motor of supplementary unloading mechanism, the heating chamber that the rectangle passageway passed the degasification jar extends to inside the degasification jar.
The invention has the beneficial effects that:
the invention removes chlorine, sulfur dioxide and hydrogen chloride gas in an alkyl sulfonyl chloride mixture by a method combining mechanical stirring and hot gas leaching, and moves a material spraying mechanism leftwards and rightwards through a mechanical structure design to intercept solid impurities of the alkyl sulfonyl chloride mixture at the upper end of a filter screen, the filter screen is in a convex design to facilitate cleaning of the impurities The degassing process for producing the sodium hexadecyl sulfonate has the characteristics of convenience in blanking, safety in use and the like, has great application value in the process of producing the sodium hexadecyl sulfonate, is simple in process from the reaction sulfonylation reaction of heavy oil, chlorine and sulfur dioxide to the saponification reaction of alkyl sulfonyl chloride to the production of the sodium alkyl sulfonate, and has high product purity and high yield, thereby showing that the process has great application value in the process of industrially producing the sodium hexadecyl sulfonate.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view of the structure of a degassing apparatus according to the present invention;
FIG. 2 is a schematic view showing the internal structure of the degassing apparatus of the present invention;
fig. 3 is a schematic structural view of an auxiliary blanking mechanism in the present invention.
The reference numerals in the drawings represent the following:
1. a first support plate; 11. a connecting member; 12. a universal wheel; 2. a degassing tank; 21. a feed pipe; 22. a feed valve; 23. an air exhaust pipe; 24. an air extraction valve; 25. a discharge pipe; 26. a discharge valve; 27. a flow guide pipe; 28. a control valve; 3. an auxiliary blanking mechanism; 31. a slide bar; 32. a slider; 33. a piston head; 34. a connecting rod; 4. a second support plate; 41. a second motor; 42. a screw rod; 5. a gas storage tank; 51. a gas delivery pipe; 52. a valve; 53. a connecting pipe; 54. a gas showerhead; 55. a bronchus; 6. a third support plate; 61. a first motor; 62. a stirring shaft; 63. a first bearing sleeve; 64. a helical mixing blade; 65. a first pulley; 66. a second pulley; 67. a belt; 68. a threaded rod; 681. a third bearing sleeve; 69. a second bearing housing; 7. a filter screen; 71. a circular truncated cone; 8. distributing pipes; 81. a branch pipe; 82. a moving block; 83. and (4) a spray head.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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
A degassing process for the production of sodium hexadecylsulfonate, comprising the steps of:
adding heavy oil into a reaction kettle, introducing mixed gas consisting of chlorine and sulfur dioxide in a volume ratio of 1:2 into the reaction kettle under the illumination of ultraviolet rays, controlling the temperature in the reaction kettle to be 31 ℃, and reacting for 3 hours at a rotating speed of 100r/min to obtain an alkyl sulfonyl chloride mixture;
secondly, putting the alkyl sulfonyl chloride mixture into a degassing device from a feeding pipe 21, removing chlorine, sulfur dioxide and a byproduct hydrogen chloride gas in the alkyl sulfonyl chloride mixture through the degassing device to obtain impurity-removed alkyl sulfonyl chloride liquid, and discharging the liquid out of the degassing device through a discharging pipe 25 to obtain purified alkyl sulfonyl chloride;
thirdly, adding the purified alkyl sulfonyl chloride into a reaction tank filled with 35% sodium hydroxide solution by mass fraction, keeping the temperature of the reaction tank at 95 ℃, reacting for 1h at the rotating speed of 200r/min, wherein the molar ratio of the purified alkyl sulfonyl chloride to the sodium hydroxide is 1:2, and obtaining a mixed solution A containing sodium alkyl sulfonate after the reaction is finished;
and fourthly, adding the mixed solution A into a heat preservation cylinder, preserving heat for 4 hours at the temperature of 105 ℃, separating a lower water phase B, adding the lower water phase B into the heat preservation cylinder again, preserving heat for 8 hours at the temperature of 105 ℃, separating a lower water phase C, adding a sodium bicarbonate solution with the mass fraction of 20% into the lower water phase C, and adjusting the pH value to be 7 to obtain the sodium hexadecylsulfonate.
Example 2
A degassing process for the production of sodium hexadecylsulfonate, comprising the steps of:
adding heavy oil into a reaction kettle, introducing mixed gas consisting of chlorine and sulfur dioxide in a volume ratio of 1:2 into the reaction kettle under the illumination of ultraviolet rays, controlling the temperature in the reaction kettle to be 33 ℃, and reacting for 4 hours at a rotating speed of 150r/min to obtain an alkyl sulfonyl chloride mixture;
secondly, putting the alkyl sulfonyl chloride mixture into a degassing device from a feeding pipe 21, removing chlorine, sulfur dioxide and a byproduct hydrogen chloride gas in the alkyl sulfonyl chloride mixture through the degassing device to obtain impurity-removed alkyl sulfonyl chloride liquid, and discharging the liquid out of the degassing device through a discharging pipe 25 to obtain purified alkyl sulfonyl chloride;
thirdly, adding the purified alkyl sulfonyl chloride into a reaction tank filled with 35% sodium hydroxide solution by mass fraction, keeping the temperature of the reaction tank at 98 ℃, reacting for 1.5h under the condition of the rotating speed of 250r/min, wherein the molar ratio of the purified alkyl sulfonyl chloride to the sodium hydroxide is 1:2, and obtaining a mixed solution A containing sodium alkyl sulfonate after the reaction is finished;
and fourthly, adding the mixed solution A into a heat preservation cylinder, preserving heat for 4 hours at the temperature of 108 ℃, separating a lower water phase B, adding the lower water phase B into the heat preservation cylinder again, preserving heat for 8 hours at the temperature of 108 ℃, separating a lower water phase C, adding a sodium bicarbonate solution with the mass fraction of 20% into the lower water phase C, and adjusting the pH value to be 7 to obtain the sodium hexadecylsulfonate.
Example 3
A degassing process for the production of sodium hexadecylsulfonate, comprising the steps of:
adding heavy oil into a reaction kettle, introducing mixed gas consisting of chlorine and sulfur dioxide in a volume ratio of 1:2 into the reaction kettle under the illumination of ultraviolet rays, controlling the temperature in the reaction kettle to be 35 ℃, and reacting for 5 hours at a rotating speed of 200r/min to obtain an alkyl sulfonyl chloride mixture;
secondly, putting the alkyl sulfonyl chloride mixture into a degassing device from a feeding pipe 21, removing chlorine, sulfur dioxide and a byproduct hydrogen chloride gas in the alkyl sulfonyl chloride mixture through the degassing device to obtain impurity-removed alkyl sulfonyl chloride liquid, and discharging the liquid out of the degassing device through a discharging pipe 25 to obtain purified alkyl sulfonyl chloride;
thirdly, adding the purified alkyl sulfonyl chloride into a reaction tank filled with 35% sodium hydroxide solution by mass fraction, keeping the temperature of the reaction tank at 100 ℃, reacting for 2 hours at the rotating speed of 300r/min, wherein the molar ratio of the purified alkyl sulfonyl chloride to the sodium hydroxide is 1:2, and obtaining a mixed solution A containing sodium alkyl sulfonate after the reaction is finished;
and fourthly, adding the mixed solution A into a heat preservation cylinder, preserving heat for 4 hours at the temperature of 110 ℃, separating a lower water phase B, adding the lower water phase B into the heat preservation cylinder again, preserving heat for 8 hours at the temperature of 110 ℃, separating a lower water phase C, adding a sodium bicarbonate solution with the mass fraction of 20% into the lower water phase C, and adjusting the pH value to be 8 to obtain the sodium hexadecylsulfonate.
Referring to fig. 1-3, in the second step, the degassing device includes a first support plate 1, a degassing tank 2 and an auxiliary blanking mechanism 3, where the first support plate 1 is a rectangular plate horizontally placed, four corners of the lower end of the first support plate 1 are all fixedly provided with connecting pieces 11, each connecting piece 11 is movably connected with a universal wheel 12, the degassing tank 2 is fixedly disposed above the first support plate 1, the auxiliary blanking mechanism 3 is located at one side of the degassing tank 2 and is supported and fixed by a second support plate 4, and one end of the second support plate 4 is fixedly welded on a surface of one side of the degassing tank 2;
the upper end center position of the degassing tank 2 is fixedly provided with a feeding pipe 21, the feeding pipe 21 penetrates through the upper wall of the degassing tank 2 and extends into the degassing tank 2, the feeding pipe 21 is fixedly provided with a feeding valve 22, the feeding pipe 21 is a plastic hose, one side of the feeding pipe 21 is fixedly provided with an exhaust pipe 23, one end of the exhaust pipe 23 penetrates through the upper wall of the degassing tank 2 and extends into the degassing tank 2, the exhaust pipe 23 is fixedly provided with an exhaust valve 24, the bottom end of the exhaust pipe 23 is fixedly provided with an activated carbon adsorption plate, the lower end center position of the degassing tank 2 is fixedly provided with a discharge pipe 25, the discharge pipe 25 penetrates through the first support plate 1 and extends to the lower end of the first support plate 1, the discharge pipe 25 is fixedly provided with a discharge valve 26, the degassing tank 2 is divided into an inner layer and an outer layer, the bottom end structure of the inner layer of the degassing tank 2 is arc-shaped, a heating cavity is arranged between the inner layer and the outer layer of the degassing tank 2, one end of a guide pipe 27 penetrates through the outer wall of the degassing tank 2 and extends into the heating cavity, the guide pipe 27 is fixedly provided with a control valve 28, hot oil or hot water is injected into the guide pipe 27, and the hot oil or hot water enters the heating cavity of the degassing tank 2 to provide heating conditions of constant temperature water bath or constant temperature oil bath for the degassing tank 2;
a third supporting plate 6 is fixedly installed on one side of the outer wall of the degassing tank 2, a first motor 61 is fixedly arranged on the third supporting plate 6, the output end of the first motor 61 is fixedly connected with a stirring shaft 62 through a coupler, one end of the stirring shaft 62 penetrates through the heating cavity and extends into the degassing tank 2, a first bearing sleeve 63 is fixedly sleeved on the stirring shaft 62, the first bearing sleeve 63 is hermetically connected with the inner wall and the outer wall of the degassing tank 2, a plurality of spiral stirring blades 64 are fixedly connected on the stirring shaft 62, a first belt pulley 65 is sleeved on one side of the stirring shaft 62 close to the first motor 61, a second belt pulley 66 is arranged above the first belt pulley 65, the first belt pulley 65 is connected with the second belt pulley 66 through a belt 67, the second belt pulley 66 is sleeved on a threaded rod 68, one end of the threaded rod 68 penetrates through and extends into the degassing tank 2, a second bearing sleeve 69 is sleeved on one end of the threaded rod 68 close to the heating cavity of the second belt pulley 66, the second bearing sleeve 69 is connected with the inner wall and the outer wall of the degassing tank 2 in a sealing manner, one end of the threaded rod 68, which is far away from the second belt pulley 66, is rotatably arranged in the third bearing sleeve 681, the third bearing sleeve 681 is welded on the inner wall of the degassing tank 2, the threaded rod 68 is provided with reverse threads which extend towards two ends by taking the middle as a starting point, the threaded rod 68 is in threaded sleeve connection with two material spraying mechanisms, each material spraying mechanism comprises a branch pipe 81 and a spray head 83, the branch pipe 81 is fixedly connected and communicated with the spray head 83, the branch pipe 81 is fixedly connected and communicated with a moving block 82, the moving block 82 is in threaded sleeve connection with the threaded rod 68, threads matched with the threaded rod 68 are arranged in the moving block 82, the upper end of the branch pipe 81 is fixedly connected and communicated with the material distributing pipe 8, and the middle part of the material distributing pipe 8 is fixedly connected and communicated with the feed pipe 21;
a filter screen 7 is fixedly arranged below the material spraying mechanism, the filter screen 7 is supported and fixed by a circular table 71, and the circular table 71 is fixedly arranged on the inner wall of the degassing tank 2;
an air injection mechanism is fixedly arranged below the stirring shaft 62, the air injection mechanism comprises a branch air pipe 55, the branch air pipe 55 is fixedly arranged at the upper end of an air injection head 54, the branch air pipe 55 is communicated with the air injection head 54, the lower end of the air injection head 54 is fixedly connected and communicated with a connecting pipe 53, one end, far away from the air injection head 54, of the connecting pipe 53 is fixedly connected and communicated with an air pipe 51, one end, far away from the air injection head 54, of the air pipe 51 penetrates through the inner wall and the outer wall of the degassing tank 2 to extend to the outside of the degassing tank 2 and is communicated with an air storage tank 5, and a valve 52 is fixedly arranged on the air pipe 51;
a second motor 41 is fixedly arranged on the second supporting plate 4, the output end of the second motor 41 is fixedly connected with a screw rod 42 through a coupler, one end of the screw rod 42 penetrates through the outer wall of the box body of the auxiliary blanking mechanism 3 and is in threaded connection with the middle part of the slide rod 31, a sliding chute 35 is formed in the upper end and the lower end of the box body of the auxiliary blanking mechanism 3, slide blocks 32 are fixedly connected to the upper end and the lower end of the slide rod 31, one side of the slide rod 31 is fixedly connected with a piston head 33 through two connecting rods 34, the size of the piston head 33 is matched with that of the box body of the auxiliary blanking mechanism 3, a rectangular channel is formed in one end of the auxiliary blanking mechanism 3, which is far away from the second motor 41, and the rectangular channel penetrates through the heating cavity of the degassing tank 2 and extends into the degassing tank 2;
the working method of the degassing device comprises the following steps:
opening a feed valve 22, putting an alkyl sulfonyl chloride mixture into a degassing tank 2 from a feed pipe 21, starting a first motor 61, driving a stirring shaft 62 to rotate by the first motor 61, stirring the alkyl sulfonyl chloride mixture by a spiral stirring blade 64 on the stirring shaft 62, driving a second belt pulley 66 to rotate by a first belt pulley 65 on the stirring shaft 62 through a belt 67, further driving a threaded rod 68 to rotate, enabling a spraying mechanism on the threaded rod 68 to move left and right, enabling the alkyl sulfonyl chloride mixture to uniformly penetrate through a filter screen 7 and enter the bottom of the degassing tank 2, then opening a control valve 28, introducing hot oil with the temperature of 60-65 ℃ into a flow guide pipe 27, opening a valve 52, introducing hydrogen or other gases into the degassing tank 2, after 10-15min reaction, opening an extraction valve 24, connecting an extraction pipe 23 with an exhaust fan, extracting the gas from the interior of the degassing tank 2, and after finishing the extraction, the second motor 41 is started, the second motor 41 drives the piston head 33 in the auxiliary blanking mechanism 3 to move back and forth to extrude gas in the degassing tank 2, and materials in the degassing tank 2 are more easily discharged from the discharge pipe 25 by utilizing the change of pressure intensity.
The foregoing is illustrative and explanatory only of the present invention, and it is intended that the present invention cover modifications, additions, or substitutions by those skilled in the art, without departing from the spirit of the invention or exceeding the scope of the claims.
Claims (3)
1. A degassing process for producing sodium hexadecylsulfonate, which is characterized by comprising the following steps:
step one, adding heavy oil into a reaction kettle, introducing mixed gas consisting of chlorine and sulfur dioxide in a volume ratio of 1:2 into the reaction kettle under the illumination of ultraviolet rays, controlling the temperature in the reaction kettle to be 33 +/-2 ℃, and reacting for 3-5 hours under the condition of a rotation speed of 100 plus-one materials of 200r/min to obtain an alkyl sulfonyl chloride mixture;
secondly, putting the alkyl sulfonyl chloride mixture into a degassing device from a feeding pipe (21), removing chlorine, sulfur dioxide and a byproduct hydrogen chloride gas in the alkyl sulfonyl chloride mixture through the degassing device to obtain impurity-removed alkyl sulfonyl chloride liquid, and discharging the liquid out of the degassing device through a discharging pipe (25) to obtain purified alkyl sulfonyl chloride;
thirdly, adding purified alkyl sulfonyl chloride into a reaction tank filled with 35% sodium hydroxide solution by mass fraction, keeping the temperature of the reaction tank at 95-100 ℃, and reacting for 1-2h under the condition of the rotation speed of 200-;
fourthly, adding the mixed solution A into a heat preservation cylinder, preserving heat for 4 hours at the temperature of 105-;
in the second step, the degassing device comprises a first supporting plate (1), a degassing tank (2) and an auxiliary blanking mechanism (3), a feeding pipe (21) is fixedly arranged at the upper end center position of the degassing tank (2), the feeding pipe (21) penetrates through the upper wall of the degassing tank (2) and extends to the inside of the degassing tank (2), a feeding valve (22) is fixedly arranged on the feeding pipe (21), the feeding pipe (21) is a plastic hose, an exhaust pipe (23) is fixedly arranged on one side of the feeding pipe (21), one end of the exhaust pipe (23) penetrates through the upper wall of the degassing tank (2) and extends to the inside of the degassing tank (2), an exhaust valve (24) is fixedly arranged on the exhaust pipe (23), an activated carbon adsorption plate is fixedly arranged at the bottom end of the exhaust pipe (23), a discharging pipe (25) is fixedly arranged at the lower end center position of the degassing tank (2), the discharging pipe (25) penetrates through the first supporting plate (1) and extends to the lower end of the first supporting plate (1), a discharge valve (26) is fixedly arranged on the discharge pipe (25), the degassing tank (2) is divided into an inner layer and an outer layer, the bottom end of the inner layer of the degassing tank (2) is in an arc shape, a heating cavity is arranged between the inner layer and the outer layer of the degassing tank (2), one end of a guide pipe (27) penetrates through the outer wall of the degassing tank (2) and extends into the heating cavity, and a control valve (28) is fixedly arranged on the guide pipe (27);
a third support plate (6) is fixedly arranged on one side of the outer wall of the degassing tank (2), a first motor (61) is fixedly arranged on the third support plate (6), the output end of the first motor (61) is fixedly connected with a stirring shaft (62) through a coupler, one end of the stirring shaft (62) penetrates through the heating cavity and extends into the degassing tank (2), a first bearing sleeve (63) is fixedly sleeved on the stirring shaft (62), the first bearing sleeve (63) is hermetically connected with the inner wall and the outer wall of the degassing tank (2), a plurality of spiral stirring blades (64) are fixedly connected on the stirring shaft (62), a first belt pulley (65) is sleeved on one side of the stirring shaft (62) close to the first motor (61), a second belt pulley (66) is arranged above the first belt pulley (65), the first belt pulley (65) is connected with the second belt pulley (66) through a belt (67), the second belt pulley (66) is sleeved on a threaded rod (68), one end of a threaded rod (68) penetrates through the heating cavity and extends to the inside of the degassing tank (2), one end, close to a second belt pulley (66), of the threaded rod (68) is sleeved with a second bearing sleeve (69), the second bearing sleeve (69) is in sealing connection with the inner wall and the outer wall of the degassing tank (2), one end, far away from the second belt pulley (66), of the threaded rod (68) is rotatably arranged inside a third bearing sleeve (681), the third bearing sleeve (681) is welded on the inner wall of the degassing tank (2), reverse threads which extend towards two ends by taking the middle as a starting point are arranged on the threaded rod (68), two material spraying mechanisms are sleeved on the threaded rod (68) in a threaded manner and comprise a branch pipe (81) and a spray head (83), the branch pipe (81) is fixedly connected with the spray head (83) and communicated with the spray head (82), a branch pipe (82) is fixedly sleeved on the threaded rod (68), threads matched with the threaded rod (68) are arranged in the moving block (82), the upper end of the branch pipe (81) is fixedly connected and communicated with the material distributing pipe (8), and the middle part of the material distributing pipe (8) is fixedly connected and communicated with the feeding pipe (21);
a filter screen (7) is fixedly arranged below the material spraying mechanism, the filter screen (7) is supported and fixed by a circular table (71), and the circular table (71) is fixedly arranged on the inner wall of the degassing tank (2);
the fixed jet-propelled mechanism that sets up in (mixing) shaft (62) below, the jet-propelled mechanism includes bronchus (55), bronchus (55) is fixed to be set up in jet head (54) upper end, and bronchus (55) are linked together with jet head (54), jet head (54) lower extreme and connecting pipe (53) fixed connection and communicate with each other, the one end and gas-supply pipe (51) fixed connection and the communication of jet head (54) are kept away from in connecting pipe (53), the one end that gas-supply pipe (51) were kept away from jet head (54) is passed the outside that degasification jar (2) inside and outside wall extended to degasification jar (2) and is linked together with gas holder (5), fixed valve (52) that are provided with on gas-supply pipe (51).
2. The degassing process for producing sodium hexadecylsulfonate according to claim 1, wherein the first supporting plate (1) is a rectangular plate horizontally and transversely placed, the four corners of the lower end of the first supporting plate (1) are fixedly provided with connecting pieces (11), each connecting piece (11) is movably connected with a universal wheel (12), the degassing tank (2) is fixedly arranged above the first supporting plate (1), the auxiliary blanking mechanism (3) is positioned at one side of the degassing tank (2) and is supported and fixed by the second supporting plate (4), and one end of the second supporting plate (4) is fixedly welded on one side surface of the degassing tank (2).
3. The degassing process for producing the sodium hexadecyl sulfonate according to claim 2, wherein a second motor (41) is fixedly arranged on the second supporting plate (4), the output end of the second motor (41) is fixedly connected with a screw rod (42) through a coupler, one end of the screw rod (42) penetrates through the outer wall of a box body of the auxiliary blanking mechanism (3) to be in threaded connection with the middle part of the sliding rod (31), the upper end and the lower end of the box body of the auxiliary blanking mechanism (3) are provided with sliding grooves (35), the upper end and the lower end of the sliding rod (31) are fixedly connected with sliding blocks (32), one side of the sliding rod (31) is fixedly connected with a piston head (33) through two connecting rods (34), the size of the piston head (33) is matched with the box body of the auxiliary blanking mechanism (3), and one end of the auxiliary blanking mechanism (3) far away from the second motor (41) is provided with a rectangular channel, the rectangular channel extends through the heating chamber of the degassing tank (2) to the interior of the degassing tank (2).
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| CN111729565A (en) * | 2020-06-29 | 2020-10-02 | 江西国化实业有限公司 | Mixing arrangement that medical treatment chemical industry liquid raw materials used |
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| US4687649A (en) * | 1983-09-09 | 1987-08-18 | Babcock-Hitachi Kabushiki Kaisha | Flue gas desulfurization process |
| CN103304451A (en) * | 2013-05-13 | 2013-09-18 | 台州市前进化工有限公司 | Preparation method of aromatic hydrocarbon sulfonyl chloride derivative |
| CN104415580A (en) * | 2013-08-27 | 2015-03-18 | 丹阳市助剂化工厂有限公司 | Method and device for removing hydrogen chloride and residual chlorine from liquid chlorinated paraffin |
| CN104998534A (en) * | 2015-06-26 | 2015-10-28 | 潜江海为化学科技有限公司 | Recovery method for sulfonyl chloride chlorination reaction tail gas |
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| CN111729565A (en) * | 2020-06-29 | 2020-10-02 | 江西国化实业有限公司 | Mixing arrangement that medical treatment chemical industry liquid raw materials used |
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Denomination of invention: A degassing process for producing sodium hexadecyl sulfonate Effective date of registration: 20230628 Granted publication date: 20220607 Pledgee: Industrial and Commercial Bank of China Limited Hexian sub branch Pledgor: ANHUI HAISHUN CHEMICAL CO.,LTD. Registration number: Y2023980046237 |
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Granted publication date: 20220607 Pledgee: Industrial and Commercial Bank of China Limited Hexian sub branch Pledgor: ANHUI HAISHUN CHEMICAL CO.,LTD. Registration number: Y2023980046237 |