CN116854646B - Environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one - Google Patents
Environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one Download PDFInfo
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- CN116854646B CN116854646B CN202310818617.3A CN202310818617A CN116854646B CN 116854646 B CN116854646 B CN 116854646B CN 202310818617 A CN202310818617 A CN 202310818617A CN 116854646 B CN116854646 B CN 116854646B
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- kettle body
- vertical shaft
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- benzisothiazolin
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- DMSMPAJRVJJAGA-UHFFFAOYSA-N benzo[d]isothiazol-3-one Chemical compound C1=CC=C2C(=O)NSC2=C1 DMSMPAJRVJJAGA-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000001308 synthesis method Methods 0.000 title claims abstract description 20
- 239000007789 gas Substances 0.000 claims abstract description 105
- 238000006243 chemical reaction Methods 0.000 claims abstract description 54
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 claims abstract description 12
- NHWQMJMIYICNBP-UHFFFAOYSA-N 2-chlorobenzonitrile Chemical compound ClC1=CC=CC=C1C#N NHWQMJMIYICNBP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 239000003651 drinking water Substances 0.000 claims abstract description 4
- 235000020188 drinking water Nutrition 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 46
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 230000007246 mechanism Effects 0.000 claims description 18
- 230000005540 biological transmission Effects 0.000 claims description 15
- 238000009434 installation Methods 0.000 claims description 12
- 238000011084 recovery Methods 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 9
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 9
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 8
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 8
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 8
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- 238000004891 communication Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 239000012074 organic phase Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000010025 steaming Methods 0.000 claims description 2
- 241000883990 Flabellum Species 0.000 claims 4
- 230000008878 coupling Effects 0.000 claims 2
- 238000010168 coupling process Methods 0.000 claims 2
- 238000005859 coupling reaction Methods 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 12
- 239000002994 raw material Substances 0.000 abstract description 10
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 239000011344 liquid material Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 8
- 238000003786 synthesis reaction Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 6
- 239000002351 wastewater Substances 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000035484 reaction time Effects 0.000 abstract description 4
- 239000002912 waste gas Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 9
- -1 antiviral Substances 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- QWXYZCJEXYQNEI-OSZHWHEXSA-N intermediate I Chemical compound COC(=O)[C@@]1(C=O)[C@H]2CC=[N+](C\C2=C\C)CCc2c1[nH]c1ccccc21 QWXYZCJEXYQNEI-OSZHWHEXSA-N 0.000 description 4
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- RWZYAGGXGHYGMB-UHFFFAOYSA-N anthranilic acid Chemical compound NC1=CC=CC=C1C(O)=O RWZYAGGXGHYGMB-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- ZGRWZUDBZZBJQB-UHFFFAOYSA-N benzenecarbodithioic acid Chemical compound SC(=S)C1=CC=CC=C1 ZGRWZUDBZZBJQB-UHFFFAOYSA-N 0.000 description 2
- 238000009395 breeding Methods 0.000 description 2
- 230000001488 breeding effect Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229940035676 analgesics Drugs 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000000730 antalgic agent Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000002785 anti-thrombosis Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 239000000164 antipsychotic agent Substances 0.000 description 1
- 229940005529 antipsychotics Drugs 0.000 description 1
- 229940127217 antithrombotic drug Drugs 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 238000007040 multi-step synthesis reaction Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- RMBAVIFYHOYIFM-UHFFFAOYSA-M sodium methanethiolate Chemical compound [Na+].[S-]C RMBAVIFYHOYIFM-UHFFFAOYSA-M 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1868—Stationary reactors having moving elements inside resulting in a loop-type movement
- B01J19/1875—Stationary reactors having moving elements inside resulting in a loop-type movement internally, i.e. the mixture circulating inside the vessel such that the upwards stream is separated physically from the downwards stream(s)
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D275/00—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings
- C07D275/04—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings condensed with carbocyclic rings or ring systems
-
- 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
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses an environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one, and belongs to the technical field of synthesis of 1, 2-benzisothiazolin-3-one. The invention is used for solving the technical problems that in the prior art, the pressure of waste water and waste gas in the synthesis process of 1, 2-benzisothiazolinone is high on the aspect of environmental protection, and the difficulty of uniform mixing of gas materials and liquid materials in the reaction process is high, so that the reaction cost is not controlled, and the environmental protection synthesis method of 1, 2-benzisothiazolin-3-one comprises the following steps: 137.5g of o-chlorobenzonitrile, 400g of drinking water, 104g of 70wt% sodium hydrosulfide and 5g of catalyst were fed from a feed pipe of a reaction apparatus into a reactor having a capacity of 1L. The invention not only reduces the cost of the reaction raw materials and the production of waste gas and waste water, improves the reaction yield, but also improves the mixing effect between the gas materials and the liquid materials, reduces the reaction time and is beneficial to controlling the production cost.
Description
Technical Field
The invention relates to the technical field of synthesis of 1, 2-benzisothiazolin-3-one, in particular to an environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one.
Background
The benzisothiazolinone compounds are the most important nitrogenous and thioheterocyclic compounds, and the derivatives thereof show broad-spectrum biological activity, can be used as bactericides, antipsychotics, antiviral, antithrombotic and analgesic drugs and the like, and are widely applied to the industries of medicines, agriculture and foods. The 1, 2-benzisothiazolin-3-one has outstanding effect of inhibiting the breeding of microorganisms such as mould (fungi or bacteria) and algae in an organic medium, solves a series of problems such as mildew, fermentation, deterioration, demulsification, odor and the like of organic products caused by the breeding of the microorganisms, is widely applied to products such as latex products, water-soluble resins, coatings, acrylic acid, polymers and the like, and is an important industrial sterilization, corrosion prevention and mildew prevention agent.
In the prior art, the synthesis method of 1, 2-benzisothiazolin-3-one mainly comprises two steps, wherein one method takes o-aminobenzoic acid as a raw material to prepare dithiobenzoic acid, and then the dithiobenzoic acid is subjected to acyl chlorination, ammoniation and chlorination to prepare 1, 2-benzisothiazolinone; the other is that o-chlorobenzonitrile is taken as a raw material, and is reacted with alkane thiol and then cyclized by chlorination to prepare 1, 2-benzisothiazolinone, the alkane thiol in the prior art has higher market price and is unfavorable for reducing cost, and the alkane thiol has bad odor, extremely high requirements on transportation and use links and high requirements on environmental protection by waste gas generated in the reaction process; the existing synthesis method adopts multi-step synthesis, the post-treatment process is complex, the wastewater amount is large, and the yield is low; the reaction of gas materials and liquid materials is needed in the reaction process, the traditional reaction device can not achieve the effect of fully mixing the gas materials and the liquid materials, the reaction rate is low, and the reaction time is long.
In view of the technical drawbacks of this aspect, a solution is now proposed.
Disclosure of Invention
The invention aims to provide an environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one, which is used for solving the technical problems that in the prior art, raw alkane thiol used in the synthesis process of 1, 2-benzisothiazolinone is high in price and has malodor, the amount of waste water in the synthesis process is large, the pressure of waste water and waste gas on the environment-friendly aspect is large, and the difficulty of uniformly mixing gas materials and liquid materials in the reaction process is large, so that the contact area of the gas materials and the liquid materials is small, the reaction time is long, and the reaction cost is unfavorable to control.
The aim of the invention can be achieved by the following technical scheme:
an environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one comprises the following steps:
s1, 137.5g of o-chlorobenzonitrile, 400g of drinking water, 104g of 70wt% sodium hydrosulfide and 5g of catalyst are added into a kettle body with the capacity of 1L from a feed pipe of a reaction device, a plurality of stirring rods in the kettle body rotate, and the temperature inside the kettle body is reduced to 5-10 ℃;
s2, closing a feed pipe, vacuumizing the kettle body, adding 1mol/L hydrochloric acid 65mL into the kettle body through negative pressure suction, closing all valves outside the kettle body, opening an electromagnetic valve in a vertical shaft, conveying gas at the top of the inner side of the kettle body to the inner side of the vertical shaft by a wind collecting assembly, conveying the gas downwards by an air extracting assembly, and discharging the gas from the bottom of an installation block, so that hydrogen sulfide gas forms circulation in a reaction solution and upper air, and the temperature inside the kettle body is increased to 80-90 ℃ for 4-5 hours;
the chemical reaction involved in step S2 includes:
NaHS+HCl→H 2 S+NaCl
s3, the temperature of the kettle body is reduced to room temperature, an electromagnetic valve in a vertical shaft is closed, a valve on an exhaust pipe is opened, hydrochloric acid is added into the kettle body, the pH value of the system is regulated to be 1, stirring is carried out for 30-50min, and hydrogen sulfide generated in the kettle body is conveyed to a recovery section for recovery;
the chemical reaction involved in step S3 includes:
NaHS+HCl→H 2 S+NaCl
s4, closing all valves outside the kettle body, increasing the temperature of the kettle body to 115-125 ℃, increasing the pressure to 0.15-0.5MPa, reacting for 4-6 hours, cooling to room temperature, adding 150g of chlorobenzene into the kettle body to extract a reaction system for 2 times, merging organic phases, and drying to obtain a chlorobenzene solution;
the chemical reaction involved in step S3 includes:
s5, transferring the chlorobenzene solution to the inner side of a kettle body, rotating a plurality of stirring rods in the kettle body, reducing the temperature of the kettle body to 5-15 ℃, vacuumizing the kettle body, introducing chlorine gas into the kettle body, raising the pressure of the kettle body to 0.4-0.6MPa, reacting for 4-6h, opening an electromagnetic valve in a vertical shaft, conveying gas at the top of the inner side of the kettle body to the inner side of the vertical shaft by an air collecting assembly, conveying the gas downwards by an air extracting assembly, discharging the gas from the bottom of an installation block, circulating the chlorine gas in the reaction solution, and raising the temperature of the kettle body to 60-70 ℃;
the main chemical reactions involved in step S5 include:
s6, closing an electromagnetic valve in the vertical shaft, opening a valve on the exhaust pipe, and conveying hydrogen chloride in the kettle body to a hydrogen chloride recovery section for treatment;
s7, raising the temperature of the kettle body to 85 ℃, and decompressing and steaming to remove chlorobenzene and low-boiling-point impurities to obtain 1, 2-benzisothiazolin-3-one.
Further, the catalyst consists of tetrabutylammonium bromide and potassium iodide according to the weight ratio of 3:2.
Further, the reaction device comprises a kettle body, a vertical shaft with a hollow structure is arranged on the inner side of the kettle body, a stirring mechanism is arranged outside the vertical shaft, a wind collecting assembly for conveying gas to the inside of the vertical shaft is arranged at the top of the vertical shaft, and an air extracting assembly for conveying gas at the top of the vertical shaft to the bottom of the vertical shaft is arranged at the bottom of the vertical shaft, wherein the wind collecting assembly is in transmission connection with the vertical shaft through a speed reducing mechanism;
the air extraction assembly comprises an installation block sleeved at the bottom of the vertical shaft, an annular cavity is formed in the inner side of the installation block, a plurality of air cylinders are fixedly installed on the inner side of the annular cavity and are communicated with the inside of the vertical shaft through unidirectional air inlet pipes, air guide holes corresponding to the plurality of air cylinders are formed in the bottoms of the installation blocks, air outlet unidirectional valves are installed on the air guide holes, a driving ring is sleeved outside the plurality of air cylinders and fixedly connected with the inner wall of the kettle body through a plurality of connecting rods, and a driving groove matched with the air cylinders is formed in the inner wall of the driving ring.
Further, the inlet pipe has been cup jointed at the top of the cauldron body, and the discharging pipe has been cup jointed to the bottom of the cauldron body, and the bottom outer wall of vertical axle rotates and installs the adapter ring, and a plurality of intercommunications that are linked together with the vertical axle respectively have been seted up to the inboard of adapter ring, and the solenoid valve is installed to the vertical axle, and the solenoid valve is located the below of a plurality of intercommunications, and the blast pipe has been cup jointed to one side outer wall of adapter ring, and the blast pipe is kept away from the one end of adapter ring and is extended to the outside of the cauldron body.
Further, the stirring mechanism comprises a plurality of stirring layers and a plurality of fixed layers, the stirring layers and the fixed layers are alternately arranged, the stirring layers are formed by a plurality of stirring rods I fixedly connected to the outer portion of the vertical shaft and arranged in an annular array, and the fixed layers are formed by a plurality of stirring rods II fixedly installed on the inner wall of the kettle body.
Further, the fan collecting mechanism comprises an annular seat rotatably arranged at the top of the vertical shaft, a plurality of fan blades are fixedly connected to the top of the annular seat, a top plate is fixedly connected to the top of the plurality of fan blades, a driving motor for driving the top plate to rotate is arranged at the top of the kettle body, the plurality of fan blades are arranged in an annular array with the center of the top plate, and the plurality of fan blades are of an arc-shaped structure.
Further, the speed reducing mechanism comprises an annular cavity formed in the bottom of the annular seat and an annular plate fixedly sleeved outside the vertical shaft, a plurality of tooth grooves which are vertically arranged are formed in the inner wall of the annular cavity, an inner gear ring is fixedly connected to the top of the annular plate, an annular cover is arranged at the top of the inner gear ring, the bottom of the annular cover is fixedly connected with the top of the connecting ring, a plurality of gear sets are rotatably mounted on the top of the inner side of the annular cover, and two ends of the gear sets are meshed with the tooth grooves and the inner gear ring respectively.
Further, the gas cylinder comprises a fixed cylinder fixedly connected to the inner side wall of the annular cavity, a connecting cylinder movably sleeved on the inner side of the fixed cylinder and an end cylinder movably sleeved on the inner side of the connecting cylinder, one end of the connecting cylinder, which is positioned on the inner side of the fixed cylinder, is matched with the fixed cylinder, one end of the end cylinder, which is positioned on the inner side of the connecting cylinder, is mutually matched with the connecting cylinder, and springs are arranged on the inner sides of the fixed cylinder and the connecting cylinder.
The invention has the following beneficial effects:
1. the invention relates to an environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one, which comprises the steps of preparing an intermediate I through the reaction of o-chlorobenzonitrile and 70wt% of sodium hydrosulfide in the presence of a catalyst, hydrolyzing the intermediate I in a pressure and high-temperature environment to generate an intermediate II, introducing chlorine into a reaction system of the intermediate II, and performing cyclization reaction to obtain a product 1, 2-benzisothiazolin-3-one; compared with the traditional process for preparing the 1, 2-benzisothiazolin-3-one, in the process for preparing the 1, 2-benzisothiazolin-3-one, sodium hydrosulfide is used for replacing the traditional alkane thiols raw material, the redundant hydrogen sulfide generated in the reaction process can be recycled, the waste water generated in the reaction process is less, the environmental protection pressure is reduced, the sodium hydrosulfide raw material is selected, the folding price is 4000 yuan/ton, the cheapest sodium methyl mercaptide in alkane thiols is 20000 yuan/ton, the price of the raw material is obviously reduced, the solid content of the sodium hydrosulfide is 70%, the liquid content is 20%, the transportation is convenient, the safety and the environmental protection pressure is low; the yield of the 1, 2-benzisothiazolin-3-one product obtained by the synthesis method provided by the invention reaches 95%, and the synthesis yield of the 1, 2-benzisothiazolin-3-one is effectively improved.
2. According to the reaction device provided by the invention, through the mutual matching of the kettle body, the vertical shaft, the wind collecting assembly, the air extracting assembly and the stirring mechanism, the fan blades and the annular seat on the wind collecting assembly can convey the gas raw materials in the kettle body to the vertical shaft in the synthesis process of 1, 2-benzisothiazolin-3-one, and through the matching of the electromagnetic valve and the adapter ring arranged on the vertical shaft and the exhaust pipe, the gas in the kettle body can be conveyed to the bottom of the kettle body or the outside of the kettle body, so that the gas in the kettle body can be selectively conveyed to adapt to the treatment requirements of the gas in different reaction stages in the synthesis process of 1, 2-benzisothiazolin-3-one; the vertical shaft is in transmission connection with the wind collecting assembly through a speed reducing mechanism arranged on the adapter ring, the exhaust pipe plays a limiting role, and the rotation of the adapter ring is avoided, so that the wind collecting assembly can drive the vertical shaft to synchronously rotate while working; the mounting block, the gas cylinder, the transmission ring, the gas inlet one-way pipe and the gas guide hole on the gas extraction assembly are mutually matched, so that the gas cylinder continuously generates compression deformation and resumes the deformation process when the mounting block rotates, gas is discharged from the bottom of the mounting block, the phenomenon that the gas cannot be discharged due to the plugging of the gas guide hole by liquid pressure is avoided, the gas in the kettle body is continuously conveyed to the inside of the vertical shaft by the gas collection assembly, the gas material can be ensured to be filled with the gas cylinder rapidly when the gas cylinder resumes the deformation, and the circulation rate of the gas material in a liquid reaction solution is further improved; the internal cavity of the kettle body is divided into a plurality of layers by the plurality of fixed layers on the stirring mechanism, the layers are mutually connected in series, gas overflows upwards in the form of bubbles under the action of buoyancy, the stirring layer and the fixed layers form a barrier, a plurality of stirring rods similar to a spindle-shaped structure rotate, the bubbles are dispersed while being disturbed to move, the mixing uniformity between the gas and liquid materials is improved, the time of the bubbles remained in the liquid is prolonged, the reaction rate is further improved, the reaction time is shortened, and the cost in the aspect of control is facilitated.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic perspective view of the whole reaction apparatus of the present invention;
FIG. 2 is a schematic diagram showing a schematic cross-sectional front view of a reaction apparatus according to the present invention;
FIG. 3 is an enlarged schematic view of the structure of FIG. 2A according to the present invention;
FIG. 4 is a schematic top cross-sectional view of the mounting block of the present invention;
FIG. 5 is a schematic view of a wind collecting assembly according to the present invention;
FIG. 6 is a schematic view of the structure of the speed reducing mechanism of the present invention after being unfolded;
FIG. 7 is a schematic view of the connection structure of the vertical shaft, stirring rod I and the mounting block in the invention.
In the figure: 100. a kettle body; 101. a feed pipe; 102. a discharge pipe; 200. a vertical axis; 201. a stirring rod I; 202. a stirring rod II; 203. a linking ring; 204. a communication hole; 205. an exhaust pipe; 300. an annular seat; 301. a fan blade; 302. a top plate; 303. a driving motor; 400. an annular chamber; 401. tooth slots; 402. an annular plate; 403. an inner gear ring; 404. an annular cover; 405. a gear set; 500. a mounting block; 501. an annular chamber; 502. a fixed cylinder; 503. a connecting cylinder; 504. an end cylinder; 505. a one-way air inlet pipe; 506. an air guide hole; 507. a drive ring; 508. a transmission groove; 509. and (5) connecting a rod.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1-3, a reaction device for an environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one in this embodiment includes a kettle body 100, a hollow vertical shaft 200 is mounted on the inner side of the kettle body 100, a feed pipe 101 is sleeved on the top of the kettle body 100, a discharge pipe 102 is sleeved on the bottom of the kettle body 100, a connection ring 203 is rotatably mounted on the outer wall of the bottom of the vertical shaft 200, a plurality of communication holes 204 respectively communicated with the vertical shaft 200 are formed on the inner side of the connection ring 203, an electromagnetic valve is mounted on the vertical shaft 200 and located below the plurality of communication holes 204, an exhaust pipe 205 is sleeved on the outer wall of one side of the connection ring 203, and one end of the exhaust pipe 205, which is far away from the connection ring 203, extends to the outside of the kettle body 100.
Install valve (not shown) on blast pipe 205, if the gas in the cauldron body 100 moves downwards through the top of vertical axis 200, close the solenoid valve on the vertical axis 200, open the valve on blast pipe 205, conveniently discharge the outside of cauldron body 100 with gas in the cauldron body 100, close the valve on blast pipe 205, open the solenoid valve on the vertical axis 200, then can downwards export gas, discharge from the bottom of vertical axis 200, form the circulation in the gas in the inboard top cavity of cauldron body 100 and the inboard reaction system of cauldron body 100, the effectual mixed effect between gas material and the liquid reaction system that has improved.
Example 2
Referring to fig. 2, 3, 5 and 6, a reaction device for an environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one in this embodiment includes a wind collecting assembly mounted at the top of a vertical shaft 200 for conveying gas into the vertical shaft 200, the wind collecting assembly includes an annular seat 300 rotatably mounted at the top of the vertical shaft 200, a plurality of fan blades 301 are fixedly connected at the top of the annular seat 300, a top plate 302 is fixedly connected at the top of the plurality of fan blades 301, a driving motor 303 for driving the top plate 302 to rotate is mounted at the top of the kettle body 100, the plurality of fan blades 301 are arranged in an annular array with the center of the top plate 302, and the plurality of fan blades 301 are all in an arc structure;
the annular seat 300 is of a round table-shaped structure with a cavity in the center of the top, the annular seat 300 is driven to synchronously rotate through the transmission of the fan blades 301 while the top plate 302 rotates, the top of the vertical shaft 200 extends to the top of the annular seat 300 and is flush with the bottom surface of the cavity in the top of the annular seat 300, the driving motor 303 drives the top plate 302 to rotate, the top plate 302, the fan blades 301 and the annular seat 300 are driven to synchronously rotate, the fan blades 301 of the arc-shaped structure disturb the gas atmosphere inside the kettle body 100 and attract gas inside the kettle body 100 to collect to the inside of the vertical shaft 200 when rotating, the electromagnetic valve in the vertical shaft 200 is closed, the gas inside the kettle body 100 can be conveyed to the exhaust pipe 205 when the valve on the exhaust pipe 205 is opened, the electromagnetic valve on the exhaust pipe 205 is opened, the gas can be discharged from the bottom of the vertical shaft 200 when the pressure at the bottom of the vertical shaft 200 is smaller, and the effect of promoting the gas to circulate in the liquid reaction system is achieved.
The wind collecting assembly is in transmission connection with the vertical shaft 200 through a speed reducing mechanism, the speed reducing mechanism comprises an annular cavity 400 formed in the bottom of the annular seat 300 and an annular plate 402 fixedly sleeved outside the vertical shaft 200, a plurality of tooth grooves 401 which are vertically formed in the inner wall of the annular cavity 400 are formed in the top of the annular plate 402, an inner gear ring 403 is fixedly connected to the top of the annular plate 402, an annular cover 404 is arranged at the top of the inner gear ring 403, the bottom of the annular cover 404 is fixedly connected with the top of the connecting ring 203, a plurality of gear sets 405 are rotatably mounted at the top of the inner side of the annular cover 404, and two ends of the gear sets 405 are meshed with the tooth grooves 401 and the inner gear ring 403 respectively.
When the annular seat 300 rotates, the exhaust pipe 205 not only plays a role in exhausting, but also plays a role in positioning and fixing, and the adapter ring 203 is prevented from synchronously rotating along with the vertical shaft 200, so that the annular seat 300 rotates and simultaneously is driven to rotate through a plurality of gear sets 405, the annular gear 403 is driven to rotate, the annular plate 402 is driven to be grabbed, and the vertical shaft 200 is further rotated.
Example 3
Referring to fig. 2, 4 and 7, the reaction device for the environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one of the present embodiment includes an air extraction assembly mounted at the bottom of the vertical shaft 200 for delivering the gas at the top of the vertical shaft 200 to the bottom thereof, the air extraction assembly includes a mounting block 500 sleeved at the bottom of the vertical shaft 200, an annular chamber 501 is provided at the inner side of the mounting block 500, a plurality of gas cylinders are fixedly mounted at the inner side of the annular chamber 501, the plurality of gas cylinders are all communicated with the inside of the vertical shaft 200 through a unidirectional gas inlet pipe 505, gas guide holes 506 corresponding to the plurality of gas cylinders are provided at the bottom of the plurality of mounting blocks 500, a gas outlet unidirectional valve is mounted on the gas guide holes 506, a driving ring 507 is sleeved outside the plurality of gas cylinders, the driving ring 507 is fixedly connected with the inner wall of the kettle body 100 through a plurality of connecting rods 509, and a driving groove 508 matched with the gas cylinders is provided on the inner wall of the driving ring 507;
when the vertical shaft 200 rotates, the mounting block 500 is driven to rotate, the mounting block 500 and the transmission ring 507 rotate relatively, so that the gas cylinder is continuously subjected to compression deformation and recovery deformation, when the gas cylinder is compressed, gas in the gas cylinder is output from the bottom of the mounting block 500 through the gas hole 506, when the gas cylinder recovers deformation, the gas collected at the inner top of the kettle body 100 flows to the inner side of the gas cylinder rapidly under the combined action of the suction effect of the gas cylinder and the gas transmission effect of the gas collection assembly in the vertical shaft 200, the inner cavity of the gas cylinder is filled, the mounting block 500 is in a hemispherical structure, when the gas is discharged from the gas hole 506, the gas moves upwards along the bottom inclined plane of the mounting block 500, the gas is uniformly distributed in the kettle body 100, and the top of the mounting block 500 is in a conical structure, so that the collection of reaction liquid at the top of the mounting block 500 can be avoided during discharging.
The gas cylinder comprises a fixed cylinder 502 fixedly connected to the inner side wall of the annular cavity 501, a connecting cylinder 503 movably sleeved on the inner side of the fixed cylinder 502 and an end cylinder 504 movably sleeved on the inner side of the connecting cylinder 503, one end of the connecting cylinder 503 positioned on the inner side of the fixed cylinder 502 is matched with the fixed cylinder 502, one end of the end cylinder 504 positioned on the inner side of the connecting cylinder 503 is matched with the connecting cylinder 503, and springs are arranged on the inner sides of the fixed cylinder 502 and the connecting cylinder 503.
The inner walls of the fixed cylinder 502 and the connecting cylinder 503 are respectively provided with a containing groove (not shown) horizontally arranged along the length direction, a plurality of springs are respectively arranged on the inner sides of the containing grooves, one ends of the springs close to the end cylinder 504 are respectively provided with connecting sliding blocks (not shown), one ends of the connecting sliding blocks extend to the outer parts of the containing grooves and are respectively fixedly connected with the bottom of one end of the connecting cylinder 503 or the end cylinder 504 close to the fixed cylinder 502, the bottom of the transmission groove 508 is of an arc-shaped structure, one end of the end cylinder 504 far away from the fixed cylinder 502 is provided with an arc-shaped surface matched with the transmission groove 508, when the mounting block 500 rotates, the plurality of gas cylinders and the transmission ring 507 relatively move, when the mounting block 500 is positioned on the inner side of the transmission groove 508, the mounting block 500 rotates clockwise, the end cylinder 504 and the connecting cylinder 503 are pushed to move towards the fixed cylinder 502, when the top of the end cylinder 504 is abutted against the bottom of the transmission groove 508, the plurality of springs are compressed completely, gas in the gas cylinder is output from the bottom of the mounting block 500, the gas cylinder enters the adjacent transmission groove 508 from the inner side, the inner side of the gas cylinder is sucked under the action of the springs, and the gas is quickly sucked in, and the gas is deformed, and the gas is quickly sucked.
Example 4
Referring to fig. 2 and 7, a reaction device for an environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one in this embodiment includes a stirring mechanism mounted outside a vertical shaft 200, the stirring mechanism includes a plurality of stirring layers and a plurality of fixing layers, the plurality of stirring layers and the plurality of fixing layers are alternately arranged, the stirring layers are composed of a plurality of stirring rods I201 fixedly connected outside the vertical shaft 200 and arranged in an annular array, and the fixing layers are composed of a plurality of stirring rods II 202 fixedly mounted on the inner wall of the kettle body 100.
The stirring rods 201 rotate synchronously along with the rotation of the vertical shaft 200, so that the reaction system in the kettle body 100 is fully and uniformly mixed, the internal cavity of the kettle body 100 is divided into a plurality of layers of mutually communicated serial structures by the fixing layers, gas output from the bottom of the mounting block 500 overflows upwards in the form of bubbles under the action of buoyancy, the stirring layers and the fixing layers form a barrier, the residence time of the bubbles in the reaction system is prolonged, the stirring rods 201 rotate and disturb the movement of the bubbles and scatter the bubbles, the mixing uniformity between the gas and liquid materials is improved, the cross section of the stirring rods 201 is similar to a fusiform structure, the upper end and the lower end of the stirring rods 201 are provided with arc surfaces which are symmetrically arranged, the left end and the right end of the stirring rods 201 are respectively in an included angle of 45 degrees, the stirring rods 201 rotate and simultaneously play a role of turbulent flow, the residence time of the bubbles in the liquid is prolonged, and the reaction rate is further improved.
Example 5
Referring to fig. 1-7, the environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one in the embodiment comprises the following steps:
s1, 137.5g of o-chlorobenzonitrile, 400g of drinking water, 104g of 70wt% sodium hydrosulfide, 3g of tetrabutylammonium bromide and 2g of potassium iodide are added into a kettle body 100 with the capacity of 1L from a feed pipe 101 of a reaction device, a gas collecting assembly rotates and is driven by a speed reducing mechanism to drive a vertical shaft 200 to rotate, so that a plurality of stirring rods I201 in the kettle body 100 are driven to rotate, a reaction system in the kettle body is uniformly stirred, and the internal temperature of the kettle body 100 is reduced to 7.5 ℃;
s2, closing a feed pipe 101, vacuumizing a kettle body 100, adding 1mol/L hydrochloric acid 65mL into the kettle body 100 in a negative pressure material sucking mode, closing all valves outside the kettle body 100, opening an electromagnetic valve in a vertical shaft 200, conveying gas at the top of the inner side of the kettle body 100 to the inner side of the vertical shaft 200 by a wind collecting assembly, mutually matching the wind collecting assembly with a gas exhausting assembly, conveying the gas downwards, and discharging the gas from the bottom of an installation block 500, so that hydrogen sulfide gas circulates in a reaction solution and upper air, mutually matching a plurality of stirring rods I201 and II 202, scattering rising bubbles, prolonging the retention time of the bubbles in liquid, raising the temperature inside the kettle body 100 to 85 ℃, reacting for 4.5h, and detecting that the residue of raw materials is 0.4 by HPLC;
s3, the temperature of the kettle body 100 is reduced to room temperature, an electromagnetic valve in a vertical shaft 200 is closed, a valve on an exhaust pipe 205 is opened, hydrochloric acid is added into the kettle body 100, the pH=1 of the system is regulated, stirring is carried out for 40min, hydrogen sulfide generated in the kettle body 100 is conveyed to a recovery section for recovery, sodium hydroxide solution is used for recovering the hydrogen sulfide gas in the recovery section, sodium hydrosulfide is prepared, and the sodium hydrosulfide is recycled;
s4, closing all valves outside the kettle body 100, increasing the temperature of the kettle body 100 to 120 ℃, increasing the pressure to 0.3MPa, reacting for 5 hours, detecting the residue of the raw material intermediate I to 0.6 percent by HPLC, cooling to room temperature, adding 150g of chlorobenzene into the kettle body 100 to extract a reaction system for 2 times, merging organic phases, transferring the organic phases to the inner side of the kettle body 100, increasing the temperature of the kettle body 100 to 120 ℃, and separating water in the reaction system by a water separator to obtain a chlorobenzene solution;
s5, reducing the temperature of the kettle body 100 to 10 ℃, vacuumizing the kettle body 100, introducing chlorine into the kettle body 100, increasing the pressure of the kettle body 100 to 0.5MPa, reacting for 5 hours, detecting that the residue of the raw material intermediate II is 0.4%, opening an electromagnetic valve in a vertical shaft 200, conveying gas at the top of the inner side of the kettle body 100 to the inner side of the vertical shaft 200 by an air collecting assembly, conveying the gas downwards by an air extracting assembly, discharging the gas from the bottom of an installation block 500, mutually matching a plurality of stirring rods I201 and a stirring rod II 202, scattering the ascending chlorine bubbles, and prolonging the retention time of the bubbles in liquid;
s6, closing an electromagnetic valve in the vertical shaft 200, opening a valve on the exhaust pipe 205, and conveying hydrogen chloride in the kettle body 100 to a hydrogen chloride recovery section for treatment, wherein chlorine gas is respectively absorbed by water and strong sodium oxide;
s7, raising the temperature of the kettle body 100 to 85 ℃, and evaporating chlorobenzene and low-boiling-point impurities under reduced pressure to obtain 143.5g of 1, 2-benzisothiazolin-3-one, wherein the yield is 95%.
After the intermediate in the reaction process is purified, the intermediate structure generated in the reaction process is detected and analyzed by a mass spectrometer, and specific detection and analysis data are as follows:
intermediate I: m/z 135.0203 (100.0%), 136.0207 (7.6%), 137.0098 (4.5%);
intermediate II: m/z 153.0268 (100.0%), 154.0312 (7.6%), 155.0198 (4.5%);
the product is: m/z 151.0105 (100.0%), 152.0098 (7.6%), 153.0102 (4.5%).
The foregoing is merely illustrative and explanatory of the invention, as it is well within the scope of the invention as claimed, as it relates to various modifications, additions and substitutions for those skilled in the art, without departing from the inventive concept and without departing from the scope of the invention as defined in the accompanying claims.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (4)
1. An environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one is characterized by comprising the following steps:
s1, 137.5g of o-chlorobenzonitrile, 400g of drinking water, 104g of 70wt% sodium hydrosulfide and 5g of catalyst are added into a kettle body (100) with the capacity of 1L from a feed pipe (101) of a reaction device, a plurality of stirring rods I (201) in the kettle body (100) rotate, the internal temperature of the kettle body (100) is reduced to 5-10 ℃, wherein the catalyst consists of tetrabutylammonium bromide and potassium iodide according to the weight ratio of 3:2;
s2, closing a feed pipe (101), vacuumizing a kettle body (100), adding 100mL of hydrochloric acid into the kettle body (100) through negative pressure suction, closing all valves outside the kettle body (100), opening electromagnetic valves in a vertical shaft (200), conveying gas at the inner side top of the kettle body (100) to the inner side of the vertical shaft (200) by an air collecting assembly, conveying the gas downwards by an air extracting assembly, and discharging the gas from the bottom of an installation block (500) so that hydrogen sulfide gas forms circulation in a reaction solution and upper air, wherein the temperature inside the kettle body (100) is raised to 80-90 ℃ and the reaction lasts for 4-5 hours;
s3, the temperature of the kettle body (100) is reduced to room temperature, an electromagnetic valve in a vertical shaft (200) is closed, a valve on an exhaust pipe (205) is opened, hydrochloric acid is added into the kettle body (100), the pH value of the system is regulated to be 1, stirring is carried out for 30-50min, and hydrogen sulfide generated in the kettle body (100) is conveyed to a recovery section for recovery;
s4, closing all valves outside the kettle body (100), increasing the temperature of the kettle body (100) to 115-125 ℃, increasing the pressure to 0.15-0.5MPa, reacting for 4-6 hours, cooling to room temperature, adding 150g of chlorobenzene into the kettle body (100) to extract a reaction system for 2 times, merging organic phases, and drying to obtain a chlorobenzene solution;
s5, transferring chlorobenzene solution to the inner side of a kettle body (100), rotating a plurality of stirring rods I (201) in the kettle body (100), reducing the temperature of the kettle body (100) to 5-15 ℃, vacuumizing the kettle body (100), introducing chlorine into the kettle body (100), raising the pressure of the kettle body (100) to 0.4-0.6MPa, reacting for 4-6h, opening an electromagnetic valve in a vertical shaft (200), conveying gas at the top of the inner side of the kettle body (100) to the inner side of the vertical shaft (200) by an air collecting assembly, conveying the gas downwards by an air extracting assembly, discharging the gas from the bottom of an installation block (500), forming chlorine circulation in the reaction solution, and raising the temperature of the kettle body (100) to 60-70 ℃;
s6, closing an electromagnetic valve in the vertical shaft (200), opening a valve on the exhaust pipe (205), and conveying hydrogen chloride in the kettle body (100) to a hydrogen chloride recovery section for treatment;
s7, raising the temperature of the kettle body (100) to 85 ℃, and decompressing and steaming to remove chlorobenzene and low-boiling-point impurities to obtain 1, 2-benzisothiazolin-3-one;
the reaction device comprises a kettle body (100), wherein a vertical shaft (200) with a hollow structure is arranged on the inner side of the kettle body (100), a stirring mechanism is arranged outside the vertical shaft (200), a wind collecting assembly for conveying gas to the inside of the vertical shaft (200) is arranged at the top of the vertical shaft (200), and a gas extracting assembly for conveying the gas at the top of the vertical shaft (200) to the bottom of the vertical shaft is arranged at the bottom of the vertical shaft (200), wherein the wind collecting assembly is in transmission connection with the vertical shaft (200) through a speed reducing mechanism;
the air extraction assembly comprises an installation block (500) sleeved at the bottom of a vertical shaft (200), an annular cavity (501) is formed in the inner side of the installation block (500), a plurality of air cylinders are fixedly arranged on the inner side wall of the annular cavity (501), the air cylinders are communicated with the inside of the vertical shaft (200) through one-way air inlet pipes (505), air guide holes (506) which are arranged corresponding to the air cylinders are formed in the bottoms of the installation blocks (500), an air outlet one-way valve is arranged on the air guide holes (506), a plurality of driving rings (507) are sleeved outside the air cylinders, the driving rings (507) are fixedly connected with the inner wall of the kettle body (100) through a plurality of connecting rods (509), and driving grooves (508) matched with the air cylinders are formed in the inner wall of the driving rings (507);
the novel kettle is characterized in that a feeding pipe (101) is sleeved at the top of the kettle body (100), a discharging pipe (102) is sleeved at the bottom of the kettle body (100), a connecting ring (203) is rotatably installed on the outer wall of the bottom of the vertical shaft (200), a plurality of communication holes (204) which are respectively communicated with the vertical shaft (200) are formed in the inner side of the connecting ring (203), an electromagnetic valve is installed on the vertical shaft (200), the electromagnetic valve is located below the plurality of communication holes (204), an exhaust pipe (205) is sleeved on the outer wall of one side of the connecting ring (203), and one end, far away from the connecting ring (203), of the exhaust pipe (205) extends to the outside of the kettle body (100);
the wind collection subassembly is including rotating annular seat (300) of installing at vertical axis (200) top, the top rigid coupling of annular seat (300) has a plurality of flabellum (301), and a plurality of the top rigid coupling of flabellum (301) has roof (302), be used for driving roof (302) pivoted driving motor (303) are installed at the top of cauldron body (100), a plurality of flabellum (301) are annular array setting with the centre of a circle of roof (302), and a plurality of flabellum (301) are arc structure.
2. The environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one according to claim 1, wherein the stirring mechanism comprises a plurality of stirring layers and a plurality of fixing layers, the stirring layers and the fixing layers are alternately arranged, the stirring layers are composed of a plurality of stirring rods I (201) fixedly connected to the outside of a vertical shaft (200) and arranged in an annular array, and the fixing layers are composed of a plurality of stirring rods II (202) fixedly arranged on the inner wall of a kettle body (100).
3. The environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one according to claim 1, wherein the speed reducing mechanism comprises an annular chamber (400) arranged at the bottom of an annular seat (300) and an annular plate (402) fixedly sleeved outside a vertical shaft (200), a plurality of vertically arranged tooth grooves (401) are formed in the inner wall of the annular chamber (400), an inner gear ring (403) is fixedly connected to the top of the annular plate (402), an annular cover (404) is arranged at the top of the inner gear ring (403), the bottom of the annular cover (404) is fixedly connected with the top of a connecting ring (203), a plurality of gear sets (405) are rotatably arranged at the inner top of the annular cover (404), and two ends of each gear set (405) are respectively meshed with the tooth grooves (401) and the inner gear ring (403).
4. The environment-friendly synthesis method of 1, 2-benzisothiazolin-3-one according to claim 1, wherein the gas cylinder comprises a fixed cylinder (502) fixedly connected to the inner side wall of the annular chamber (501), a connecting cylinder (503) movably sleeved on the inner side of the fixed cylinder (502) and an end cylinder (504) movably sleeved on the inner side of the connecting cylinder (503), one end of the connecting cylinder (503) positioned on the inner side of the fixed cylinder (502) is matched with the fixed cylinder (502), one end of the end cylinder (504) positioned on the inner side of the connecting cylinder (503) is matched with the connecting cylinder (503), and springs are arranged on the inner sides of the fixed cylinder (502) and the connecting cylinder (503).
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