CN107739325A - A kind of equipment and technique of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram - Google Patents

A kind of equipment and technique of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram Download PDF

Info

Publication number
CN107739325A
CN107739325A CN201710868007.9A CN201710868007A CN107739325A CN 107739325 A CN107739325 A CN 107739325A CN 201710868007 A CN201710868007 A CN 201710868007A CN 107739325 A CN107739325 A CN 107739325A
Authority
CN
China
Prior art keywords
tank
pipeline
pump
continuous production
liquid storage
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201710868007.9A
Other languages
Chinese (zh)
Other versions
CN107739325B (en
Inventor
徐均
苗静
徐清华
薛香菊
周福鹏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHANDONG SUNSINE CHEMICAL CO Ltd
Original Assignee
SHANDONG SUNSINE CHEMICAL CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SHANDONG SUNSINE CHEMICAL CO Ltd filed Critical SHANDONG SUNSINE CHEMICAL CO Ltd
Priority to CN201710868007.9A priority Critical patent/CN107739325B/en
Publication of CN107739325A publication Critical patent/CN107739325A/en
Application granted granted Critical
Publication of CN107739325B publication Critical patent/CN107739325B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C333/00Derivatives of thiocarbamic acids, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
    • C07C333/14Dithiocarbamic acids; Derivatives thereof
    • C07C333/30Dithiocarbamic acids; Derivatives thereof having sulfur atoms of dithiocarbamic groups bound to other sulfur atoms
    • C07C333/32Thiuramsulfides; Thiurampolysulfides

Abstract

The invention discloses a kind of equipment and technique of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram, it is related to fine chemical product technical field.The present invention includes solvent tank, dimethylamine tank, curing canister, the solvent tank, dimethylamine tank, curing canister is connected by the upper end charging aperture of pipeline and blending tank respectively, the lower end discharging opening of the blending tank is connected by the lower end charging aperture of pipeline and tower reactor, also include dioxygen water pot, the lower end discharging opening of the dioxygen water pot is pumped into device by segmentation and is connected with the side wall of tower reactor, the discharging opening on the tower reactor top is connected by pipeline with reacting the upper end charging aperture of liquid storage tank, the lower end of the reaction liquid storage tank is connected by pipeline with reverse washing device.The present invention being capable of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram.

Description

A kind of equipment of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram and Technique
Technical field
The present invention relates to fine chemical product technical field, more particularly, to a kind of continuous production thiofide two Vulcanize the equipment and technique of tetra methylthiuram.
Background technology
Tetramethylthiuram disulfide is vulcanization of rubber ultra fast accelerator, is thiazole accelerator, can be with other accelerator It is used in combination, is generally used in combination with accelerant MBT.Mainly for the manufacture of tire, the inner tube of a tyre, rubber overshoes, medical supplies, cable, industrial rubber system Product etc., it can also be used to bactericide and insecticide agriculturally, also act as lube oil additive.
The production method of vulcanization accelerator tetramethylthiuram disulfide has three kinds substantially:Sodium salt chlorine oxidation process, sodium salt Hydrogen peroxide oxidation method and the direct hydrogen peroxide oxidation method of organic solvent.At present, sodium salt chlorine oxidation process can produce in process of production Substantial amounts of brine waste and the tail gas containing chlorine and dimethylamine, it is difficult to handle, heavy contamination, processing cost is high, and chlorine Gas belongs to toxic articles, safety and environmentally friendly hidden danger in use be present;And although sodium salt hydrogen peroxide oxidation method solves tail gas Problem, but due to saliferous in waste water, it is difficult to biochemical treatment.Both the above production technology is intermittent production technology, intervalization Product quality has differences between production batch, and production efficiency is low, and equipment is more, and investment is big.
The content of the invention
In order to make up the deficiencies in the prior art, the invention provides a kind of continuous production vulcanization of rubber accelerant disulfide four The equipment and technique of methyl thiuram.
The technical solution adopted by the present invention is:
A kind of equipment of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram, including solvent tank 1, dimethylamine tank 2, Curing canister 3, the solvent tank 1, dimethylamine tank 2, curing canister 3 pass through the upper endfeed of pipeline and blending tank 4 respectively Mouth connection, the lower end discharging opening of the blending tank 4 are connected by pipeline with the lower end charging aperture of tower reactor 5, in addition to double Oxygen water pot 6, the lower end discharging opening of the dioxygen water pot 6 are pumped into device 7 by segmentation and are connected with the side wall of tower reactor 5, The discharging opening on the top of tower reactor 5 is connected by pipeline with reacting the upper end charging aperture of liquid storage tank 8, the reaction solution The lower end of storage tank 8 is connected by pipeline with reverse washing device 9.
Preferably, some distributors 51 are provided with the tower reactor 5;The segmentation, which is pumped into device 7, to be included and dioxygen The dioxygen water pump 71 that the lower end discharging opening of water pot 6 is connected, the dioxygen water pump 71 connects some branch pipes 72 by pipeline, described Branch pipe 72 is consistent with the quantity of distributor 51, and the branch pipe 72 is connected with distributor 51 respectively.
Preferably, dioxygen water flow valve group 10 is equipped with the branch pipe 72, the dioxygen water-carrying capacity positioned at the top Valve group 10 is provided with dual control regulating valve, and redox potential meter 11, the oxidation-go back are provided with the tower reactor 5 Former current potential analyzer 11 electrically connects with dual control regulating valve.
Preferably, the reverse washing device 9 includes fixed mount 91, and the lower section of the fixed mount 91 is provided with rinse bath 92, The upper end of the fixed mount 91 is provided with left carrying roller 93, right carrying roller 94 and the collecting tank between left carrying roller 93 and right carrying roller 94 95, the right carrying roller 94 is drive roll, and right carrying roller 94 is driven by motor;The left end of the fixed mount 91, right-hand member, lower end are equipped with Guide roller 96, around being equipped with endless filter belt 97 on the left carrying roller 93, right carrying roller 94 and guide roller 96, water in the collecting tank 95 It is flat to be provided with vacuum pan 98, from left to right by being longitudinally provided with some zone isolation plates 99 in the vacuum pan 98, the region every Collecting tank 95 is divided from plate 99 and is located at and reaction liquid storage tank 8 lower end for some collecting bins 910, the collecting bin 910 of the leftmost side The lower section for the pipeline being connected, leftmost side the and adjacent thereto lower end of the collecting bin 910 are respectively connected with mother liquor tank 911;Its The lower end of the remaining collecting bin 910 is all connected with washing lotion tank 912, and the lower end of the washing lotion tank 912 connects water pump by pipeline 913, the water pump 913 connects circulation pipe 914, and the free end of the circulation pipe 914 is respectively positioned on the top of left side collecting bin 910, The top of the collecting bin 910 of the rightmost side is additionally provided with water-supply-pipe 915.
Preferably, the left end of the collecting tank 95 is provided with seal closure 12, the endless filter belt 97 horizontal through seal closure 12, with The lower end for the pipeline that reaction liquid storage tank 8 lower end is connected is penetrated in seal closure 12.
Preferably, the solvent tank 1, dimethylamine tank 2, curing canister 3 connect respectively solvent pump 13, diformazan amine pump 14, Carbon disulfide pump 15, the solvent pump 13, diformazan amine pump 14, carbon disulfide pump 15 connect solvent flux valve group 16, diformazan respectively Amine flow valve group 17, carbon disulfide flow valve group 18, the solvent flux valve group 16, dimethylamine flow valve group 17, carbon disulfide Flow valve group 18 connects static mixer 19 by pipeline, and the static mixer 19 connects blending tank 4 by pipeline.
A kind of technique using equipment continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram as described above, Comprise the following steps:
1)Organic solvent, dimethylamine, carbon disulfide are distinguished into continuous conveying to blending tank 4 to mix;
2)Mixed homogeneous phase solution is continuously pumped into tower reactor 5 from the bottom of tower reactor 5 and is pumped into dress with segmented Put the 7 hydrogen peroxide reactions being pumped into tower reactor 5;
3)Top overflow of the reacted material through tower reactor 5 reacts the material in liquid storage tank 8 to reacting in liquid storage tank 8 When building up to the middle part of reaction liquid storage tank 8, start to carry out material reverse to the reverse blowing of washing device 9, reverse washing device 9 Washing, completes continuous separation of solid and liquid;
4)Solid drying tetramethylthiuram disulfide finished product.
Preferably, step 1)Middle organic solvent, carbon disulfide, dimethylamine are respectively by solvent pump 13, diformazan amine pump 14, two sulphur Change carbon pump 15 and be first pumped into static mixer 19, then entered again by pipeline in blending tank 4 and mixed.
Preferably, step 2)In, detected using redox potential meter 11 to whether reaction reaches terminal, When detecting that reaction reaches terminal, redox potential meter 11 automatically controls dual control regulating valve closure.
Preferably, step 3)In, when reacting the build up of material in liquid storage tank 8 to the middle part for reacting liquid storage tank 8, reaction solution Storage tank 8 starts the top blowing of collecting bin 910 to the leftmost side, and endless filter belt 97 rotates under the drive of right carrying roller 94, realizes Separation of solid and liquid, then using the filter residue on the drag flight descaling endless filter belt 97 being provided with right-hand member guide roller 96, filter residue is cleared up The cleaned groove 92 of endless filter belt 97 in cleaning fluid cleaned, circulated with this, realize continuous separation of solid and liquid.
Compared with prior art, its advantage is the present invention:
1st, the equipment utilization employed in the present invention, solvent tank, dimethylamine tank, curing canister can be utilized to realize to blending tank Interior continuous feed, successive reaction then is realized using tower reactor, finally realize continuous solid-liquid point using reverse washing device From so as to realize the function of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram;Moreover, dioxygen in the present invention Water, which by segmentation is pumped into device and is pumped into tower reactor and mixed homogeneous phase solution and reacts, ensures that the abundant of chemical reaction Carry out;
2nd, the terminal of reaction is detected in the present invention using redox potential meter, material peroxidating can be prevented again Or dysoxidation and cause product quality to fluctuate;
3rd, the present invention in counter flow washing device setting, realize continuous separation of solid and liquid;
4th, in the present invention static mixer setting, the ion reaction of dimethylamine and carbon disulfide can be achieved, and realize homogeneous Mixing.
Brief description of the drawings
Fig. 1 is the structural representation of the technique of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram of the present invention Figure;
Fig. 2 is the section view figure structure schematic representation of reverse washing device in Fig. 1.
In figure:1st, solvent tank, 2, dimethylamine tank, 3, curing canister, 4, blending tank, 5, tower reactor, 6, hydrogen peroxide Tank, 7, segmentation be pumped into device, 8, reaction liquid storage tank, 9, reverse washing device, 10, dioxygen water flow valve group, 11, oxidationreduction Potential measurement instrument, 12, seal closure, 13, solvent pump, 14, diformazan amine pump, 15, carbon disulfide pump, 16, solvent flux valve group, 17, Dimethylamine flow valve group, 18, carbon disulfide flow valve group, 19, static mixer;
51st, distributor, 52, temperature-reducing coil, 53, turbine stirring device, 54, chuck;
71st, dioxygen water pump, 72, branch pipe;
91st, fixed mount, 92, rinse bath, 93, left carrying roller, 94, right carrying roller, 95, collecting tank, 96, guide roller, 97, circulating filtration Band, 98, vacuum pan, 99, zone isolation plate, 910, collecting bin, 911, mother liquor tank, 912, washing lotion tank, 913, water pump, 914, circulation Pipe, 915, water-supply-pipe.
Embodiment
As shown in Figure 1, 2, a kind of equipment of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram, including it is molten Agent tank 1, dimethylamine tank 2, curing canister 3, solvent tank 1, dimethylamine tank 2, curing canister 3 pass through pipeline and blending tank respectively 4 upper end charging aperture connection, the lower end discharging opening of blending tank 4 are connected by pipeline with the lower end charging aperture of tower reactor 5, also Including dioxygen water pot 6, the lower end discharging opening of dioxygen water pot 6 is pumped into device 7 by segmentation and is connected with the side wall of tower reactor 5 Logical, the discharging opening on the top of tower reactor 5 is connected by pipeline with reacting the upper end charging aperture of liquid storage tank 8, reacts liquid storage tank 8 Lower end be connected by pipeline with reverse washing device 9.
Some distributors 51 are provided with tower reactor 5, are additionally provided with temperature-reducing coil 52, upper rotating turbine stirring device 53;Chuck 54 is additionally provided with outside tower reactor 5.
Segmentation is pumped into the dioxygen water pump 71 that device 7 includes being connected with the lower end discharging opening of dioxygen water pot 6, dioxygen water pump 71 Some branch pipes 72 are connected by pipeline, branch pipe 72 is consistent with the quantity of distributor 51, and branch pipe 72 is connected with distributor 51 respectively.
Dioxygen water flow valve group 10 is equipped with branch pipe 72, the dioxygen water flow valve group 10 positioned at the top is provided with dual control Regulating valve, tower reactor 5 is interior to be provided with redox potential meter 11, and redox potential meter 11 is adjusted with dual control Valve electrically connects.
Reverse washing device 9 includes fixed mount 91, and the lower section of fixed mount 91 is provided with rinse bath 92, and the upper end of fixed mount 91 is set There are left carrying roller 93, right carrying roller 94 and the collecting tank 95 between left carrying roller 93 and right carrying roller 94, right carrying roller 94 is drive roll, right Carrying roller 94 is driven by motor, and the left end of fixed mount 91, right-hand member, lower end are equipped with guide roller 96, left carrying roller 93, right carrying roller 94 and is led It is horizontal in collecting tank 95 to be provided with vacuum pan 98 around being equipped with endless filter belt 97 on to roller 96, pass through from left to right in vacuum pan 98 Longitudinal direction is provided with some zone isolation plates 99, and zone isolation plate 99 divides collecting tank 95 for some collecting bins 910, the collection of the leftmost side Storehouse 910 is under the lower section for the pipeline being connected with reaction liquid storage tank 8 lower end, collecting bin 910 leftmost side and adjacent thereto End is respectively connected with mother liquor tank 911;The lower end of remaining collecting bin 910 is all connected with washing lotion tank 912, and the lower end of washing lotion tank 912 passes through Pipeline connects water pump 913, and water pump 913 connects circulation pipe 914, and the free end of circulation pipe 914 is respectively positioned on the upper of left side collecting bin 910 Side, the function of inversely eluting is realized, the top of the collecting bin 910 of the rightmost side is additionally provided with water-supply-pipe 915.
The left end of collecting tank 95 is provided with seal closure 12, and endless filter belt 97 is horizontal through seal closure 12, with reaction liquid storage tank 8 lower end The lower end for the pipeline being connected is penetrated in seal closure 12.
Solvent tank 1, dimethylamine tank 2, curing canister 3 connect solvent pump 13, diformazan amine pump 14, carbon disulfide pump respectively 15, solvent pump 13, diformazan amine pump 14, carbon disulfide pump 15 connect solvent flux valve group 16, dimethylamine flow valve group 17, two respectively Nitric sulfid flow valve group 18, solvent flux valve group 16, dimethylamine flow valve group 17, carbon disulfide flow valve group 18 pass through pipeline Static mixer 19 is connected, static mixer 19 connects blending tank 4 by pipeline.
A kind of technique using equipment continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram as above, including Following steps:
1)Organic solvent in solvent tank 1, the dimethylamine in dimethylamine tank 2, the carbon disulfide in curing canister 3 is sharp respectively Static mixer 19 is first continuously pumped into solvent pump 13, diformazan amine pump 14, carbon disulfide pump 15, is then entered again by pipeline and mixed Close in tank 4 and mix;Wherein, the organic solvent and the volume ratio of dimethylamine being pumped into blending tank 4 remain 3-15:1;It is pumped into mixed Close the dimethylamine in tank 4, the mol ratio of carbon disulfide remains 0.8-1.2:1;
2)Mixed homogeneous phase solution is continuously pumped into tower reactor 5 from the bottom of tower reactor 5 and is pumped into dress with segmented The 7 hydrogen peroxide reactions being pumped into tower reactor 5 are put, reaction temperature is 30-60 DEG C;Meanwhile determined using oxidation-reduction potentials Instrument 11 detects to whether reaction reaches terminal, and when detecting that reaction reaches terminal, redox potential meter 11 is certainly Dynamic control dual control regulating valve closure;Wherein, the dimethylamine and the mol ratio of hydrogen peroxide being pumped into per hour in tower reactor 5 be 1:1.0-1.5;
3)Top overflow of the reacted material through tower reactor 5 reacts the material in liquid storage tank 8 to reacting in liquid storage tank 8 When building up to the middle part of reaction liquid storage tank 8, start to the reverse blowing of washing device 9, the material that reacted liquid storage tank 8 is released falls The endless filter belt 97 of the top of collecting bin 910 of the leftmost side, endless filter belt 97 rotate under the drive of right carrying roller 94, collecting tank The vacuum pan 98 being provided with 95 makes to produce subnormal ambient in collecting tank 95, accelerates the speed of separation of solid and liquid, through the leftmost side and and its The mother liquor that adjacent collecting bin 910 is collected is flowed into mother liquor tank 911, is returned through the mother liquor that mother liquor tank 911 is collected into distillation process Dimethylamine is received, and the cleaning solution collected through washing lotion tank 912 then enters circulation pipe 914, then through the collecting bin to the left of circulation pipe 914 910 top tapping, is filtered using endless filter belt 97, realize reverse elution, finally using being provided with right-hand member guide roller 96 Solid on drag flight descaling endless filter belt 97, the cleaning fluid cleared up in the cleaned groove 92 of endless filter belt 97 of solid are carried out Cleaning, is circulated with this, repeats separation of solid and liquid;
4)The solid being cleaned out is dried using drying plant produces tetramethylthiuram disulfide finished product, realizes serialization Produce vulcanization of rubber accelerant disulfide tetra methylthiuram.
In process of production, embodiment one:According to above-mentioned continuous production vulcanization of rubber accelerant disulfide tetramethyl Step used by the technique of base thiuram, by solvent with 1700L/h, dimethylamine is with 290L/h, and carbon disulfide is with 140L/h's Flow is pumped into blending tank 4 through static mixer 19, and tower reactor 5 is pumped into measuring pump in the case where keeping liquid level certain, Hydrogen peroxide in dioxygen water pot 6 divides three sections to be pumped into tower reactor 5 by 128L/h flow, keeps 35 DEG C of reaction temperature, reaction After end, the solid isolated through reverse washing device 9 is dried using drying plant, quantitative 8 hours materials, altogether output 2.15 tons of the output of vulcanization of rubber accelerant disulfide tetra methylthiuram, the rate of recovery is counted as 97% using dimethylamine, and obtained The just fusing point of vulcanization of rubber accelerant disulfide tetra methylthiuram finished product is 142.1 DEG C, purity 99.0%.
Embodiment two:Technique according to above-mentioned continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram Used step, by solvent with 2000L/h, dimethylamine is with 280L/h, and carbon disulfide is with 140L/h flow through static mixing Device 19 is pumped into blending tank 4, and tower reactor 5 is pumped into measuring pump in the case where keeping liquid level certain, double in dioxygen water pot 6 Oxygen water divides three sections to enter tower reactor by 140L/h flow, after keeping 45 DEG C of reaction temperature, reaction to terminate, through reverse elution The solid that device 9 is isolated is dried using drying plant, quantitative 8 hours materials, altogether output thiofide two Vulcanize 2.04 tons of the output of tetra methylthiuram, the rate of recovery is counted as 96% using dimethylamine, and obtained thiofide two The just fusing point for vulcanizing tetra methylthiuram finished product is 142.5 DEG C, purity 99.2%.

Claims (10)

  1. A kind of 1. equipment of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram, it is characterised in that:Including solvent Tank(1), dimethylamine tank(2), curing canister(3), the solvent tank(1), dimethylamine tank(2), curing canister(3)Lead to respectively Piping and blending tank(4)The connection of upper end charging aperture, the blending tank(4)Lower end discharging opening pass through pipeline and tower reaction Device(5)The connection of lower end charging aperture, in addition to dioxygen water pot(6), the dioxygen water pot(6)Lower end discharging opening pass through radially split pump Enter device(7)With tower reactor(5)Side wall be connected, the tower reactor(5)The discharging opening on top by pipeline with React liquid storage tank(8)Upper end charging aperture be connected, the reaction liquid storage tank(8)Lower end pass through pipeline and reverse washing device (9)It is connected.
  2. 2. the equipment of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram according to claim 1, it is special Sign is:The tower reactor(5)It is interior to be provided with some distributors(51);The segmentation is pumped into device(7)Including with hydrogen peroxide Tank(6)The dioxygen water pump that is connected of lower end discharging opening(71), the dioxygen water pump(71)Some branch pipes are connected by pipeline (72), the branch pipe(72)With distributor(51)Quantity is consistent, and the branch pipe(72)Respectively with distributor(51)It is connected.
  3. 3. the equipment of the continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram according to claim requirement 2, It is characterized in that:The branch pipe(72)On be equipped with dioxygen water flow valve group(10), the dioxygen water-carrying capacity positioned at the top Valve group(10)It is provided with dual control regulating valve, the tower reactor(5)It is interior to be provided with redox potential meter(11), it is described Redox potential meter(11)Electrically connected with dual control regulating valve.
  4. 4. the equipment of the continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram according to claim 1 or 3, its It is characterised by:The reverse washing device(9)Including fixed mount(91), the fixed mount(91)Lower section be provided with rinse bath (92), the fixed mount(91)Upper end be provided with left carrying roller(93), right carrying roller(94)With positioned at left carrying roller(93)With right carrying roller (94)Between collecting tank(95), the right carrying roller(94)For drive roll, driven by motor;The fixed mount(91)Left end, Right-hand member, lower end are equipped with guide roller(96), the left carrying roller(93), right carrying roller(94)And guide roller(96)On be circulated throughout around being equipped with Strainer(97), the collecting tank(95)Interior level is provided with vacuum pan(98), the vacuum pan(98)Inside pass through longitudinal direction from left to right Provided with some zone isolation plates(99), the zone isolation plate(99)By collecting tank(95)It is divided into some collecting bins(910), it is most left The collecting bin of side(910)Positioned at reacting liquid storage tank(8)The lower section for the pipeline that lower end is connected, the leftmost side and with its phase The adjacent collecting bin(910)Lower end is respectively connected with mother liquor tank(911);Remaining described collecting bin(910)Lower end be all connected with washing Flow container(912), the washing lotion tank(912)Lower end water pump is connected by pipeline(913), the water pump(913)Connection circulation Pipe(914), the circulation pipe(914)Free end be respectively positioned on left side collecting bin(910)Top, the collecting bin of the rightmost side (910)Top be additionally provided with water-supply-pipe(915).
  5. 5. the equipment of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram according to claim 4, it is special Sign is:The collecting tank(95)Left end be provided with seal closure(12), the endless filter belt(97)Horizontal through seal closure (12), with the reaction liquid storage tank(8)The lower end for the pipeline that lower end is connected penetrates seal closure(12)It is interior.
  6. 6. the equipment of the continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram according to claim requirement 5, It is characterized in that:The solvent tank(1), dimethylamine tank(2), curing canister(3)Solvent pump is connected respectively(13), diformazan amine pump (14), carbon disulfide pump(15), the solvent pump(13), diformazan amine pump(14), carbon disulfide pump(15)Solvent stream is connected respectively Measure valve group(16), dimethylamine flow valve group(17), carbon disulfide flow valve group(18), the solvent flux valve group(16), diformazan Amine flow valve group(17), carbon disulfide flow valve group(18)Static mixer is connected by pipeline(19), the static mixing Device(19)Blending tank is connected by pipeline(4).
  7. A kind of 7. work of equipment continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram using described in claim 1 Skill, it is characterised in that:Comprise the following steps:
    1)Organic solvent, dimethylamine, carbon disulfide are distinguished into continuous conveying to blending tank(4)Mixing;
    2)Mixed homogeneous phase solution is from tower reactor(5)Bottom be continuously pumped into tower reactor(5)Interior and segmented pump Enter device(7)It is pumped into tower reactor(5)Interior hydrogen peroxide reaction;
    3)Reacted material is through tower reactor(5)Top overflow to reacting liquid storage tank(8)It is interior, react liquid storage tank(8)It is interior Build up of material to reacting liquid storage tank(8)Middle part when, start to reverse washing device(9)Blowing, reverse washing device(9)It is right Material carries out counter flow washing, completes continuous separation of solid and liquid;
    4)Solid drying tetramethylthiuram disulfide finished product.
  8. A kind of 8. work of equipment continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram according to claim 7 Skill, it is characterised in that:Step 1)Middle organic solvent, carbon disulfide, dimethylamine are respectively by solvent pump(13), diformazan amine pump(14)、 Carbon disulfide pump(15)First it is pumped into static mixer(19), blending tank is then entered by pipeline again(4)Interior mixing.
  9. A kind of 9. work of equipment continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram according to claim 7 Skill, it is characterised in that:Step 2)In, utilize redox potential meter(11)Detected to whether reaction reaches terminal, When detecting that reaction reaches terminal, redox potential meter(11)Automatically control dual control regulating valve closure.
  10. 10. a kind of equipment continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram according to claim 7 Technique, it is characterised in that:Step 3)In, when reaction liquid storage tank(8)Interior build up of material is to reacting liquid storage tank(8)Middle part when, React liquid storage tank(8)Start the collecting bin to the leftmost side(910)Top blowing, endless filter belt(97)In right carrying roller(94)Band Dynamic lower rotation, realizes separation of solid and liquid, then utilizes right-hand member guide roller(96)The drag flight descaling endless filter belt that place is provided with(97)On Filter residue, cleared up the endless filter belt of filter residue(97)Cleaned groove(92)Interior cleaning fluid is cleaned, and is circulated with this, is realized Continuous separation of solid and liquid.
CN201710868007.9A 2017-09-22 2017-09-22 Equipment and process for continuously producing rubber vulcanization accelerator tetramethyl thiuram disulfide Active CN107739325B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710868007.9A CN107739325B (en) 2017-09-22 2017-09-22 Equipment and process for continuously producing rubber vulcanization accelerator tetramethyl thiuram disulfide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710868007.9A CN107739325B (en) 2017-09-22 2017-09-22 Equipment and process for continuously producing rubber vulcanization accelerator tetramethyl thiuram disulfide

Publications (2)

Publication Number Publication Date
CN107739325A true CN107739325A (en) 2018-02-27
CN107739325B CN107739325B (en) 2020-10-20

Family

ID=61236160

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710868007.9A Active CN107739325B (en) 2017-09-22 2017-09-22 Equipment and process for continuously producing rubber vulcanization accelerator tetramethyl thiuram disulfide

Country Status (1)

Country Link
CN (1) CN107739325B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112624946A (en) * 2020-12-30 2021-04-09 山东尚舜化工有限公司 Method for synthesizing promoter TMTD by continuous method
CN112645859A (en) * 2020-12-30 2021-04-13 山东尚舜化工有限公司 Novel method and equipment for improving dispersity of promoter TMTD
CN113387858A (en) * 2021-06-29 2021-09-14 山东尚舜化工有限公司 Equipment and method for continuously producing accelerant TMTD

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101717357A (en) * 2009-12-04 2010-06-02 南京工业大学 Method for preparing tetraalkyl thiuram disulphide by utilizing micro-structured reactor
CN202044945U (en) * 2011-04-21 2011-11-23 石家庄新宇三阳实业有限公司 Tower type reactor for nitric acid oxidation reaction
CN202942713U (en) * 2012-12-06 2013-05-22 福建省建阳武夷味精有限公司 Vacuum belt filter
CN204211676U (en) * 2014-09-29 2015-03-18 天津一化化工有限公司 The automated production equipment of a kind of rubber accelerator TMTD

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101717357A (en) * 2009-12-04 2010-06-02 南京工业大学 Method for preparing tetraalkyl thiuram disulphide by utilizing micro-structured reactor
CN202044945U (en) * 2011-04-21 2011-11-23 石家庄新宇三阳实业有限公司 Tower type reactor for nitric acid oxidation reaction
CN202942713U (en) * 2012-12-06 2013-05-22 福建省建阳武夷味精有限公司 Vacuum belt filter
CN204211676U (en) * 2014-09-29 2015-03-18 天津一化化工有限公司 The automated production equipment of a kind of rubber accelerator TMTD

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
MILUTIN M. MILOSAVLJEVIĆ,等: "SYNTHESIS OF TETRAALKYLTHIURAM DISULFIDES USING DIFFERENT OXIDANTS IN RECYCLING SOLVENT MIXTURE", 《CHEMICAL INDUSTRY & CHEMICAL ENGINEERING QUARTERLY》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112624946A (en) * 2020-12-30 2021-04-09 山东尚舜化工有限公司 Method for synthesizing promoter TMTD by continuous method
CN112645859A (en) * 2020-12-30 2021-04-13 山东尚舜化工有限公司 Novel method and equipment for improving dispersity of promoter TMTD
CN112624946B (en) * 2020-12-30 2023-07-14 山东尚舜化工有限公司 Method for synthesizing accelerator TMTD by continuous method
CN113387858A (en) * 2021-06-29 2021-09-14 山东尚舜化工有限公司 Equipment and method for continuously producing accelerant TMTD

Also Published As

Publication number Publication date
CN107739325B (en) 2020-10-20

Similar Documents

Publication Publication Date Title
CN107739325A (en) A kind of equipment and technique of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram
CN103466829B (en) High-concentration ammonia nitrogen waste water treatment method and system thereof
CN207153705U (en) A kind of reactor with solid-liquid separation function
CN106757294A (en) A kind of method for supplementing copper sulphate in copper plating groove
CN206793616U (en) A kind of solid-liquid reaction kettle
CN105274334B (en) A kind of method and its purification tank of solution of zinc sulfate continuous purification
CN207655079U (en) A kind of blender of paint slurry
CN207108517U (en) A kind of pyrite slag prepares the device of polymerization iron sulfate water-purifying agent
CN110743476B (en) Multifunctional calcium hydroxide preparation tank and preparation method
CN107286066A (en) A kind of technique and system of continuous production vulcanization of rubber accelerant disulfide tetra methylthiuram
CN109795996A (en) A kind of phosphoric acid by wet process vulcanization arsenic removal purification device and method
CN215626824U (en) Carborundum ring production hydrochloric acid soak device for wear-resisting axle sleeve
CN208344988U (en) Pot-type equipment is used in a kind of production of liquid detergent
CN205892924U (en) Processing apparatus who contains phenol abraum salt in mediben production process
CN204724166U (en) Air blast chemical combination bucket in electrolytic manganese process
CN210584428U (en) Copper washing tower for synthetic ammonia for chemical industry
CN210340450U (en) Calcined soda feeding device for high-salinity water treatment
CN206731084U (en) Relieving haperacidity tank
CN101456596B (en) Reactor suitable for sulphur dioxide gas leach manganese dioxide ore
CN107244654B (en) Device for separating iodine products
CN204490962U (en) Rotary type leaches unit continuously
CN206454549U (en) A kind of preparation of cerous carbonate and carbon ammonium Mead-Bauer recovery system
CN201343450Y (en) Dedicated reactor for preparing manganese sulfate solution with leached pyrolusite from sulfur dioxide gas
CN104651608B (en) Rotary continuous leaching unit and continuous countercurrent leaching method
CN109971949A (en) A kind of super leaching device and method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant