CN115710208A - Green solvent-free treatment method for thioester antioxidant - Google Patents
Green solvent-free treatment method for thioester antioxidant Download PDFInfo
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- CN115710208A CN115710208A CN202211359843.1A CN202211359843A CN115710208A CN 115710208 A CN115710208 A CN 115710208A CN 202211359843 A CN202211359843 A CN 202211359843A CN 115710208 A CN115710208 A CN 115710208A
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 27
- 150000007970 thio esters Chemical class 0.000 title claims abstract description 16
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 51
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 230000009471 action Effects 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000002378 acidificating effect Effects 0.000 claims abstract description 6
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 6
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 6
- MYWWWNVEZBAKHR-UHFFFAOYSA-N methyl 3-(3-methoxy-3-oxopropyl)sulfanylpropanoate Chemical compound COC(=O)CCSCCC(=O)OC MYWWWNVEZBAKHR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims description 63
- 238000007789 sealing Methods 0.000 claims description 55
- 239000007795 chemical reaction product Substances 0.000 claims description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 229920001971 elastomer Polymers 0.000 claims description 12
- 239000005060 rubber Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 230000005540 biological transmission Effects 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 229920000459 Nitrile rubber Polymers 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 5
- 229920001084 poly(chloroprene) Polymers 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000013013 elastic material Substances 0.000 claims description 3
- 150000002148 esters Chemical group 0.000 claims description 3
- 239000003302 ferromagnetic material Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims 3
- 238000005259 measurement Methods 0.000 claims 2
- 230000001737 promoting effect Effects 0.000 claims 2
- 230000008569 process Effects 0.000 abstract description 7
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 2
- 230000000903 blocking effect Effects 0.000 description 10
- 238000004064 recycling Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
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- 230000005291 magnetic effect Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
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- 230000002062 proliferating effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- ODJQKYXPKWQWNK-UHFFFAOYSA-L 3-(2-carboxylatoethylsulfanyl)propanoate Chemical compound [O-]C(=O)CCSCCC([O-])=O ODJQKYXPKWQWNK-UHFFFAOYSA-L 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
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- 238000002425 crystallisation Methods 0.000 description 1
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- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
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- 229920003051 synthetic elastomer Polymers 0.000 description 1
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- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
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Abstract
The application discloses a thioester antioxidant green solvent-free treatment method applied to the chemical field, in the process of preparing antioxidant DLTDP, dimethyl thiodipropionate and lauryl alcohol are used as raw materials, acidic ion exchange resin is used as a catalyst, after the reaction of the raw materials under the action of the catalyst is finished, the catalyst can be filtered and recovered for reuse, and unreacted lauryl alcohol can be distilled and recovered under the negative pressure condition.
Description
Technical Field
The application relates to the field of chemistry, in particular to a green solvent-free treatment method of thioester antioxidants.
Background
The chemical name of the antioxidant DLTDP is didecyl-glycol thiodipropionate, can be used as an auxiliary antioxidant of resins such as ABS, PVC and the like and adhesives such as natural rubber, synthetic rubber and the like, and has decomposition effect on hydroperoxide.
At present, there are two main post-processing methods after the synthesis of DLTDP: 1. the catalyst used in the reaction process is removed by adopting a method of alkali neutralization and water washing layering, the method has more complicated working procedures, and has the problems of more three wastes, high treatment cost and difficult recycling; 2. the solvent is adopted for crystallization and purification, the method is usually effectively controlled by adopting a method of reducing the temperature, the using amount of the solvent is large, and the use, the recovery and the storage of the solvent are difficult or troublesome.
Disclosure of Invention
The application aims to solve the problems of complicated working procedures, more generated three wastes, difficulty in recycling and large solvent consumption of the existing treatment method, and provides a green solvent-free treatment method of thioester antioxidants compared with the prior art, which comprises the following steps:
s1, taking dimethyl thiodipropionate and lauryl alcohol as raw materials, and taking acidic ion exchange resin as a catalyst, and carrying out ester exchange reaction on the raw materials under the action of the catalyst;
s2, after the reaction is finished, cooling the reaction product to 80-100 ℃, filtering the reaction product, filtering the catalyst and obtaining intermediate liquid;
s3, heating the intermediate solution to 170-220 ℃ under the negative pressure condition, and distilling and recovering unreacted lauryl alcohol to obtain an antioxidant product;
s4, granulating the antioxidant product by using a granulator to obtain a finished product;
when the reaction product is filtered in the S2, the reaction product can be filtered by using the beneficial production intelligent filtering device, the beneficial production intelligent filtering device comprises a filtering main pipe, a connecting cylinder and a flowmeter, the filtering main pipe is communicated with the bottom end of the connecting cylinder, the flowmeter is communicated with the top end of the connecting cylinder, a matched elastic convex filter screen is fixedly connected to the inner wall of the filtering main pipe, the elastic convex filter screen is in a shape of an upwardly convex hollow sphere, the elastic convex filter screen is made of an elastic material, an electromagnet is arranged below the elastic convex filter screen, an iron block is fixedly connected to the inner side of the elastic convex filter screen, a left side intelligent filtering controller is fixedly connected to the filtering main pipe, a secondary filter cylinder is arranged on the right side of the filtering main pipe, a flow outlet pipe is communicated with the top end of the secondary filter cylinder, the other end of the flow outlet pipe is communicated with the inside of the filtering main pipe, a backflow pipe is communicated with the inside of the filtering main pipe, a metering analysis module is arranged in the intelligent filtering controller, an automatic control module, a manual control module is electrically connected with the manual control module, the flow outlet pipe is electrically connected with the filtering main pipe, the filtering efficiency of the catalyst can be greatly improved, and the efficiency of the filtering main pipe can be greatly improved in a process of filtering process.
Optionally, a joint debugging assistant fetching component is arranged on the filtering main pipe, the joint debugging assistant fetching component comprises a regulating box fixedly connected with the filtering main pipe, a slide rail is fixedly connected to the inner wall of the bottom end of the regulating box, a joint debugging slide block is connected to the slide rail in a sliding manner and made of ferromagnetic materials, a fixed pulley is fixedly mounted in the regulating box, a sealing linkage rope is fixedly connected to one end of the joint debugging slide block and is in transmission connection with the fixed pulley, the joint debugging assistant fetching component further comprises a blocking pipe plug matched with the flow outlet pipe, the blocking pipe plug penetrates through the outer wall of the top end of the flow outlet pipe and is in sliding sealing connection with the outer wall of the flow outlet pipe, a pair of elastic pull ropes is fixedly connected between the blocking pipe plug and the inner wall of the flow outlet pipe, one end, far away from the slide rail, of the sealing linkage rope penetrates through the outer wall of the regulating box and is in sliding sealing connection with the outer wall of the flow outlet pipe, on one hand, transfer of a catalyst can be facilitated, and on the other hand, the catalyst on the other hand, can be conveniently fetched from the secondary filter screen.
Optionally, the sealing linkage rope is made of a rubber material, the rubber material is one of hydrogenated nitrile rubber and chloroprene rubber, and the rubber is soft and sealed, so that the transmission effect of the sealing linkage rope can be ensured, and the leakage of reaction products can be prevented.
Optionally, the left end of the return pipe is fixedly connected with a check valve, and the one-way conduction direction of the check valve is from right to left, so that the reaction product cannot flow into the auxiliary filter cylinder through the return pipe.
Optionally, a sealing protection box matched with the electromagnet is arranged on the outer side of the electromagnet, the sealing protection box is fixedly connected with the filtering main pipe through a pair of supporting rods, and the sealing protection box can protect the electromagnet and prevent the electromagnet from rusting and damaging.
Optionally, the bottom end of the auxiliary filter cylinder is arranged to be open, a sealing plate in threaded sealing connection with the auxiliary filter cylinder is arranged in the auxiliary filter cylinder, the sealing plate is located below the return pipe and is fixedly connected with the auxiliary filter screen through a connecting rod, a handle rod is fixedly connected to the bottom end of the sealing plate, and the auxiliary filter screen is movably connected with the auxiliary filter cylinder, so that the transfer of a catalyst can be facilitated, and the filtering efficiency can be further improved.
Optionally, the back flow is located the below of playing protruding filter screen, and the bottom of play flow tube left end flushes with the bottom of playing protruding filter screen, filters and is responsible for and connecting cylinder thread sealing connection for after filtering, rotate and filter and be responsible for and can make and filter and be responsible for and the connecting cylinder separation, thereby can be convenient for pour out and filter and be responsible for well catalyst, and then can be favorable to recycling to the catalyst.
Compare in prior art, the advantage of this application lies in:
(1) In the process of preparing the antioxidant DLTDP, dimethyl thiodipropionate and lauryl alcohol are used as raw materials, acidic ion exchange resin is used as a catalyst, after the raw materials react under the action of the catalyst, the catalyst can be filtered and recovered for reuse, and unreacted lauryl alcohol can be distilled and recovered under the negative pressure condition.
(2) Through the setting of straining the subassembly of the benefit intelligence of producing for the in-process of filtering catalyst can shift the catalyst automatically under the filterable prerequisite of not stopping, can prevent effectively that the catalyst from blockking up the protruding filter screen of bullet, leads to filtration efficiency to receive the influence, thereby can improve filtration efficiency greatly, further be applicable to large-scale industrialization volume production.
(3) Through the setting of allies oneself with the transfer and help getting the subassembly for at the in-process of filtering catalyst, in most time, the play flow tube is in the jam state, and during the transfer catalyst, goes out the flow tube and can switch on automatically, on the one hand, can be favorable to the transfer to the catalyst, and on the other hand can make the catalyst on the vice filter screen be convenient for take out.
(4) The sealing linkage rope is made of rubber material, the rubber material is one of hydrogenated nitrile rubber and chloroprene rubber, and the rubber is soft and sealed, so that the transmission effect of the sealing linkage rope can be ensured, and the leakage of reaction products can be prevented.
(5) The outside of electro-magnet is provided with assorted sealed protection box with it, and sealed protection box is responsible for fixed connection through a pair of bracing piece and filtration, and sealed protection box can play a guard action to the electro-magnet, prevents that the electro-magnet from rustting and damaging.
(6) Through the closing plate, the connecting rod, the handle bar, the antithetical couplet is transferred and is helped getting the joint setting of subassembly etc. because when the electro-magnet circular telegram, it can be stopped up by stifled pipe stopper to go out the flow tube, therefore, the staff can be when the electro-magnet is in the on state, rotate the closing plate through the handle bar, cause the closing plate to pass through the connecting rod and drive vice filter screen downstream, break away from until vice filter screen and vice straining a section of thick bamboo, can take out the catalyst on the vice filter screen, thereby can take out the catalyst under the filterable circumstances of not stopping, not only can be favorable to the transfer of catalyst, still can further improve filtration efficiency.
(7) The back flow is located the below of playing protruding filter screen, and the bottom of play flow tube left end flushes with the bottom of playing protruding filter screen, filters and is responsible for and connecting cylinder thread sealing connection for after filtering, rotate and filter and be responsible for and can make and filter and be responsible for and the connecting cylinder separation, thereby can be convenient for pour out and filter and be responsible for well catalyst, and then can be favorable to recycling to the catalyst.
Drawings
FIG. 1 is a process flow diagram of the present application;
FIG. 2 is a schematic perspective view of the apparatus for intellectual property enhancement filter according to the present application;
FIG. 3 is a schematic front view of the intellectual property filter device of the present application;
FIG. 4 is a schematic cross-sectional view of the filter manifold of the present application;
FIG. 5 is a schematic cross-sectional view of the present disclosure at the location of the protective enclosure and the pop-up screen;
FIG. 6 is a cross-sectional view of the filter cartridge of the present application;
FIG. 7 is a schematic cross-sectional view of the outlet tube of the present application;
FIG. 8 is a schematic cross-sectional view of the regulating box of the present application;
FIG. 9 is a schematic representation of a pictographic change in the filtration manifold as the reaction product is filtered using the prolific filtration device herein;
FIG. 10 is a schematic representation of a pictographic change in the effluent line during filtration of the reaction product using the prolific filter device of the present application;
FIG. 11 is a block diagram of the system architecture of the smart filter controller of the present application.
The reference numbers in the figures illustrate:
101. a main filter pipe; 102. a connecting cylinder; 103. a flow meter; 104. a convex filter screen is bounced; 105. an electromagnet; 106. an iron block; 107. an intelligent filter controller; 108. a secondary filter cartridge; 109. a flow outlet pipe; 110. a secondary filter screen; 111. a return pipe; 112. a one-way valve; 113. sealing the protection box; 114. a support bar; 115. sealing plates; 116. a connecting rod; 117. a handle bar; 201. an adjusting box; 202. a slide rail; 203. a joint adjusting slide block; 204. a fixed pulley; 205. sealing the linkage rope; 206. blocking the pipe plug; 207. an elastic pull rope.
Detailed Description
The technical solution in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application; it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all embodiments, and all other embodiments obtained by those of ordinary skill in the art without any inventive work based on the embodiments in the present application belong to the protection scope of the present application.
Example 1:
the application discloses a green solvent-free treatment method of thioester antioxidants, and the method is shown in figure 1 and comprises the following steps:
s1, taking dimethyl thiodipropionate and lauryl alcohol as raw materials, and taking acidic ion exchange resin as a catalyst, and carrying out ester exchange reaction on the raw materials under the action of the catalyst;
s2, after the reaction is finished, cooling the reaction product to 80-100 ℃, filtering the reaction product, and filtering out the catalyst to obtain intermediate liquid;
s3, heating the intermediate liquid to 170-220 ℃ under the negative pressure condition, distilling and recovering unreacted lauryl alcohol to obtain an antioxidant product;
and S4, granulating the antioxidant product by using a granulator to obtain a finished product.
In the process of preparing the antioxidant DLTDP, dimethyl thiodipropionate and lauryl alcohol are used as raw materials, acidic ion exchange resin is used as a catalyst, after the raw materials react under the action of the catalyst, the catalyst can be filtered and recovered for reuse, and unreacted lauryl alcohol can be distilled and recovered under the negative pressure condition.
Referring to fig. 2-6, 9 and 11, when the reaction product is filtered in S2, the reaction product may be filtered by using a smart filter device, the smart filter device includes a main filter pipe 101, a connecting cylinder 102 and a flowmeter 103, the main filter pipe 101 is communicated with the bottom end of the connecting cylinder 102, the flowmeter 103 is communicated with the top end of the connecting cylinder 102, a convex filter screen 104 is fixedly connected to the inner wall of the main filter pipe 101, the convex filter screen 104 is in the shape of a hollow sphere protruding upward, the convex filter screen 104 is made of an elastic material, an electromagnet 105 is disposed below the convex filter screen 104, an iron block 106 is fixedly connected to the inner side of the convex filter screen 104, a smart filter controller 107 is fixedly connected to the left side of the main filter pipe 101, an auxiliary filter cylinder 108 is disposed on the right side of the main filter pipe 101, the top end of the auxiliary filter cylinder 108 is communicated with a flow outlet pipe 109, and the other end of the flow outlet pipe 109 is communicated with the inside of the main filter pipe 101, a matched auxiliary filter screen 110 is arranged in the auxiliary filter cylinder 108, the left side of the flow outlet pipe 109 is communicated with a return pipe 111, the other end of the return pipe 111 is communicated with the inside of the filter main pipe 101, a metering analysis module, an automatic control module and a manual control module are arranged in the intelligent filter controller 107, the flowmeter 103 is electrically connected with the metering analysis module, the automatic control module is electrically connected with the manual control module, the manual control module and the automatic control module are both electrically connected with an electromagnet 105, when a reaction product is filtered by using the intelligent filter device which is beneficial to production, the electromagnet 105 can be electrified through the manual control module, the iron block 106 moves downwards under the action of magnetic attraction, the movement of the iron block 106 can drive the elastic convex filter screen 104 to deform, as shown in figure 9, the elastic convex filter screen 104 is deformed into a downward concave shape, and then the reaction product is led in from the top end of the flowmeter 103, the reaction product sequentially flows through the flow meter 103, the connecting cylinder 102 and the filtering main pipe 101, when the reaction product flows through the filtering main pipe 101, the convex filtering screen 104 can filter out the catalyst in the reaction product, and when the reaction product flows through the flow meter 103, the flow meter 103 can measure the flow of the reaction product, and transmit the measured data to the metering and analyzing module, when the flow reaches a certain value, the metering and analyzing module sends an instruction to the automatic control module, so that the automatic control module cuts off the electromagnet 105, after the electromagnet 105 is cut off, the convex filtering screen 104 can rebound to change to an upward convex shape again, so that the catalyst filtered by the convex filtering screen 104 can flow into the secondary filtering screen 108 through the flow outlet pipe 109 under the impact of the reaction product, and the secondary filtering screen 110 can filter out the catalyst again, so that the catalyst can stay on the secondary filtering screen 110, after a certain time, the automatic control module can electrify the electromagnet 105 again, so that the convex filtering screen 104 changes to a downward concave state again, so that the filtering efficiency of the convex filtering screen 104 can be changed to a downward concave state again, and the filtering screen 103 can be effectively improved at intervals, and the filtering efficiency of the catalyst can be further improved by the filtering of the filtering screen 104.
Referring to fig. 2-4, the return pipe 111 is located below the convex filter screen 104, the bottom of the left end of the outflow pipe 109 is flush with the bottom of the convex filter screen 104, and the main filtering pipe 101 is in threaded sealing connection with the connecting cylinder 102, so that after the filtering is finished, the main filtering pipe 101 is rotated to separate the main filtering pipe 101 from the connecting cylinder 102, thereby facilitating the pouring of the catalyst in the main filtering pipe 101, and further facilitating the recycling of the catalyst.
Referring to fig. 4, a check valve 112 is fixedly connected to the left end of the return pipe 111, and the one-way conduction direction of the check valve 112 is from right to left, so that the reaction product cannot flow into the auxiliary filter cartridge 108 through the return pipe 111.
Referring to fig. 4-5, a sealing protection box 113 is disposed outside the electromagnet 105, the sealing protection box 113 is fixedly connected to the main filtering pipe 101 through a pair of support rods 114, and the sealing protection box 113 can protect the electromagnet 105 to prevent the electromagnet 105 from rusting and damaging.
Referring to fig. 3-4, 7-8 and 10, a joint debugging assistant component is disposed on the main filtering pipe 101, the joint debugging assistant component includes an adjusting box 201 fixedly connected with the main filtering pipe 101, a slide rail 202 is fixedly connected to an inner wall of a bottom end of the adjusting box 201, a joint debugging slide block 203 is slidably connected to the slide rail 202, the joint debugging slide block 203 is made of ferromagnetic material, a fixed pulley 204 is fixedly installed in the adjusting box 201, a sealing link rope 205 is fixedly connected to one end of the joint debugging slide block 203, the sealing link rope 205 is in transmission connection with the fixed pulley 204, the joint debugging assistant component further includes a pipe blocking plug 206 matched with the outlet pipe 109, the pipe blocking plug 206 penetrates through and is in sliding and sealing connection with an outer wall of the outlet pipe 109, a pair of elastic pull ropes 207 is fixedly connected between the pipe blocking plug 206 and an inner wall of the outlet pipe 109, one end of the sealing link rope 205 far away from the slide rail 202 penetrates through an outer wall of the adjusting box 201 and extends to be fixedly connected with the pipe blocking plug 206, the sealing connection with an outer wall of the adjusting box 201 and an outer wall of the outlet pipe 109, through the arrangement of the joint adjusting and fetching assisting component, when the electromagnet 105 is electrified, as shown in fig. 10, the joint adjusting slide block 203 can move leftwards under the action of magnetic attraction force, therefore, the pipe plugging plug 206 can be driven to move downwards by the sealing linkage rope 205, so that the pipe plugging plug 206 plugs the outlet pipe 109, and after the electromagnet 105 is powered off, as the magnetic attraction force disappears, the pipe blocking plug 206 and the joint adjusting slide block 203 will be reset along with the rebound of the elastic pull rope 207, therefore, during the catalyst filtering process, the outlet pipe 109 is blocked for most of the time, and the outlet pipe 109 is automatically conducted when the catalyst is transferred, on the one hand, the catalyst can be transferred easily, and on the other hand, the catalyst on the secondary filter screen 110 can be taken out easily.
The sealing linkage rope 205 is made of a rubber material, the rubber material is one of hydrogenated nitrile rubber and chloroprene rubber, the rubber is soft and sealed, so that the transmission effect of the sealing linkage rope 205 can be ensured, the leakage of reaction products can be prevented, the hydrogenated nitrile rubber and the chloroprene rubber are commonly used for manufacturing a transmission belt of an automobile, the sealing linkage rope 205 with low elasticity and difficult deformation can be manufactured by adopting the two rubbers, so that the leakage of the reaction products can be further prevented, in addition, corresponding sealing measures can be arranged at the connection positions of the sealing linkage rope 205, the outflow pipe 109 and the adjusting box 201 for preventing the leakage of the reaction products, and the known technology of a person skilled in the art is omitted for further description.
Referring to fig. 6, the bottom end of the secondary filter cartridge 108 is open, a sealing plate 115 in threaded sealing connection with the secondary filter cartridge 108 is arranged in the secondary filter cartridge 108, the sealing plate 115 is located below the return pipe 111, the sealing plate 115 is fixedly connected with the secondary filter screen 110 through a connecting rod 116, the bottom end of the sealing plate 115 is fixedly connected with a handle rod 117, the secondary filter screen 110 is movably connected with the secondary filter cartridge 108, and through the combined arrangement of the sealing plate 115, the connecting rod 116, the handle rod 117, the joint adjustment and fetching-assisting component and the like, because the outlet pipe 109 is blocked by the pipe blocking plug 206 when the electromagnet 105 is energized, a worker can rotate the sealing plate 115 through the handle rod 117 when the electromagnet 105 is energized, so that the sealing plate 115 drives the secondary filter screen 110 to move downwards through the connecting rod 116 until the secondary filter screen 110 is separated from the secondary filter cartridge 108, and can fetch the catalyst on the secondary filter screen 110, thereby taking out the catalyst without stopping the filtration, not only facilitating the transfer of the catalyst, but also further improving the filtration efficiency.
The foregoing is only a preferred embodiment of the present application; the scope of protection of the present application is not limited thereto. Any person skilled in the art should also be able to cover the protection scope of the present application by the technical solutions and their modifications in the present application.
Claims (10)
1. A green solvent-free treatment method of thioester antioxidants is characterized by comprising the following steps:
s1, taking dimethyl thiodipropionate and lauryl alcohol as raw materials, and carrying out ester exchange reaction on the raw materials under the action of a catalyst;
s2, after the reaction is finished, cooling the reaction product to 80-100 ℃, filtering the reaction product, filtering the catalyst and obtaining intermediate liquid;
s3, heating the intermediate solution to 170-220 ℃ under the negative pressure condition, and distilling and recovering unreacted lauryl alcohol to obtain an antioxidant product;
s4, granulating the antioxidant product by using a granulator to obtain a finished product;
the catalyst in S1 is acidic ion exchange resin, when the reaction product is filtered in S2, the reaction product can be filtered by using a production promoting intelligent filter device, the production promoting intelligent filter device comprises a filter main pipe (101), a connecting cylinder (102) and a flowmeter (103), the filter main pipe (101) is communicated with the bottom end of the connecting cylinder (102), the flowmeter (103) is communicated with the top end of the connecting cylinder (102), the inner wall of the filter main pipe (101) is fixedly connected with an elastic convex filter screen (104) matched with the filter main pipe, the elastic convex filter screen (104) is in the shape of an upwardly convex hollow sphere, the elastic convex filter screen (104) is made of an elastic material, an electromagnet (105) is arranged below the elastic convex filter screen (104), an iron block (106) is fixedly connected to the inner side of the elastic convex filter screen (104), an intelligent filter controller (107) is fixedly connected to the left side of the filter main pipe (101), an auxiliary filter cylinder (108) is arranged on the right side of the filter main pipe (101), a flow outlet pipe (109) is arranged on the top end of the auxiliary filter cylinder (108), the other end of the flow outlet pipe (109) is communicated with the filter cylinder (109), the filter cylinder (101), the filter main pipe (111) is communicated with the auxiliary filter cylinder (108), the other end of the auxiliary flow outlet pipe (111), the filter main pipe (109), and the auxiliary flow outlet pipe (111) are communicated with the filter pipe (111), be provided with measurement analysis module, automatic control module, manual control module in intelligence is strained controller (107), flowmeter (103) are connected with measurement analysis module electricity, automatic control module is connected with manual control module electricity, manual control module, automatic control module all are connected with electro-magnet (105) electricity.
2. The green solvent-free treatment method of thioester antioxidants according to claim 1, wherein a joint adjustment pickup assembly is arranged on the main filter pipe (101), the joint adjustment pickup assembly comprises an adjusting box (201) fixedly connected with the main filter pipe (101), a slide rail (202) is fixedly connected to the inner wall of the bottom end of the adjusting box (201), a joint adjustment slider (203) is slidably connected to the slide rail (202), the joint adjustment slider (203) is made of ferromagnetic material, a fixed pulley (204) is fixedly installed in the adjusting box (201), a sealing joint rope (205) is fixedly connected to one end of the joint adjustment slider (203), and the sealing joint rope (205) is in transmission connection with the fixed pulley (204).
3. The method for green solvent-free treatment of thioester antioxidants according to claim 2, wherein the joint adjustment and extraction-assisting assembly further comprises a pipe plug (206) matched with the outflow pipe (109), the pipe plug (206) penetrates through the outer wall of the top end of the outflow pipe (109) and is connected with the outflow pipe in a sliding and sealing manner, and a pair of elastic pull ropes (207) is fixedly connected between the pipe plug (206) and the inner wall of the outflow pipe (109).
4. The method for green solvent-free treatment of thioester antioxidants according to claim 3, wherein one end of the sealed linkage rope (205) far away from the slide rail (202) penetrates through the outer wall of the regulating box (201) and extends to be fixedly connected with the pipe plugging plug (206), and the sealed linkage rope (205) is in sliding sealing connection with the outer wall of the regulating box (201) and the outer wall of the outflow pipe (109).
5. The method for green solvent-free treatment of thioester antioxidants according to claim 4, wherein said sealed linkage rope (205) is made of rubber material, said rubber material is one of hydrogenated nitrile butadiene rubber and chloroprene rubber.
6. The method for green solvent-free treatment of thioester antioxidants according to claim 1, wherein a check valve (112) is fixedly connected to the left end of the return pipe (111), and the one-way conduction direction of the check valve (112) is from right to left.
7. The method for green solvent-free treatment of thioester antioxidants according to claim 1, wherein a sealing protection box (113) matched with the electromagnet (105) is arranged outside the electromagnet (105), and the sealing protection box (113) is fixedly connected with the main filtering pipe (101) through a pair of support rods (114).
8. The method for green solvent-free treatment of thioester antioxidants according to claim 1, wherein the bottom end of the secondary filter cartridge (108) is open, a sealing plate (115) is arranged in the secondary filter cartridge (108) and is in threaded sealing connection with the secondary filter cartridge, and the sealing plate (115) is positioned below the return pipe (111).
9. The method for green solvent-free treatment of thioester antioxidants according to claim 8, wherein the sealing plate (115) is fixedly connected with the secondary filter screen (110) through a connecting rod (116), the bottom end of the sealing plate (115) is fixedly connected with a handle rod (117), and the secondary filter screen (110) is movably connected with the secondary filter cartridge (108).
10. The green solvent-free treatment method of thioester antioxidants according to claim 1, wherein the return pipe (111) is located below the convex screen (104), the bottom of the left end of the outlet pipe (109) is flush with the bottom of the convex screen (104), and the main filter pipe (101) is in threaded sealing connection with the connecting cylinder (102).
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