CN110523332B - Equipment and method for continuously producing vulcanization accelerator CBS - Google Patents
Equipment and method for continuously producing vulcanization accelerator CBS Download PDFInfo
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- CN110523332B CN110523332B CN201910870597.8A CN201910870597A CN110523332B CN 110523332 B CN110523332 B CN 110523332B CN 201910870597 A CN201910870597 A CN 201910870597A CN 110523332 B CN110523332 B CN 110523332B
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- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8362—Mixing plants; Combinations of mixers combining mixing with other treatments with chemical reactions
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- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
- B01F35/714—Feed mechanisms for feeding predetermined amounts
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- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
- B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
- B01F35/7173—Feed mechanisms characterised by the means for feeding the components to the mixer using gravity, e.g. from a hopper
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- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
- B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
- B01F35/7176—Feed mechanisms characterised by the means for feeding the components to the mixer using pumps
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- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
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- C07D277/00—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings
- C07D277/60—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings condensed with carbocyclic rings or ring systems
- C07D277/62—Benzothiazoles
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- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
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Abstract
The invention discloses equipment and a method for continuously producing a vulcanization accelerator CBS, belonging to the field of chemical production. The invention comprises an accelerant M stock bin, a water metering pump, a continuous mixing device, an M slurry metering pump, a cyclohexylamine metering pump, a hydrogen peroxide metering pump, a sodium hypochlorite metering pump, continuous reaction equipment and related pipelines. Wherein: the continuous reaction equipment has four reaction chambers, and each reaction chamber is provided with an independent stirring device. The M slurry and cyclohexylamine enter a first reaction chamber through a metering pump, hydrogen peroxide respectively enters first to third reaction chambers through the metering pump, and sodium hypochlorite enters a fourth reaction chamber through the metering pump; a discharge overflow port is arranged on the fourth reaction chamber; and the M slurry pipeline, the cyclohexylamine pipeline, the hydrogen peroxide pipeline and the sodium hypochlorite pipeline are all provided with flow regulating valve groups. The method is suitable for continuous production of the vulcanization accelerator CBS, can realize automatic control, has more stable product quality, and avoids frequent operation process of intermittent production.
Description
Technical Field
The invention relates to the field of chemical production, in particular to equipment and a method for continuously producing a vulcanization accelerator CBS.
Background
The vulcanization accelerator CBS is a slow-acting vulcanization accelerator with large consumption at home and abroad, has the advantages of excellent scorching resistance and short vulcanization time, and is mainly used for manufacturing tires, rubber tubes, rubber shoes, electric wires and the like. Meanwhile, it does not generate nitrosamine carcinogenic substances in the vulcanization process, and is one of the environment-friendly accelerators commonly used at home and abroad at present.
At present, the production of the vulcanization accelerator CBS in the industry mainly adopts kettle-type intermittent operation, and the frequent operations of feeding, reacting, discharging and the like of the intermittent reaction cause that the yield and the quality of products in each batch have large fluctuation on one hand, and increase the labor capacity of workers on the other hand, and new reaction equipment and reaction methods are required to replace the kettle-type intermittent operation in many times in the industry.
Patent CN 106800540a discloses a method for preparing rubber vulcanization accelerator CBS by using a microchannel reactor, which adopts a method of dissolving accelerator M in excess cyclohexylamine to form a solution, and feeding the solution into a microreactor for oxidation reaction, and it can be seen from the examples in the patent that the yield of the product is generally low.
Patent CN108570021A discloses a vulcanization accelerator CBS and a continuous production method thereof, the method uses a salt solution of accelerator M, an acid solution of cyclohexylamine, an oxidant and a suitable solvent as raw materials, in a continuous reactor, the vulcanization accelerator CBS is prepared, the yield of the product is improved, but the alkali for preparing the salt solution of accelerator M and the acid for preparing the acid solution of cyclohexylamine are finally present in the mother liquor in the form of salts, which increases the salt content in the wastewater, causes the wastewater to be difficult to be directly biochemically treated, and is not beneficial to environmental protection.
Disclosure of Invention
In order to make up for the defects of the prior art and solve the problems of intermittent production, large labor capacity of workers, large fluctuation of product quality among batches, low product yield and the like in the prior art, the invention provides equipment and a method for continuously producing a vulcanization accelerator CBS.
The technical scheme of the invention is as follows:
the equipment for continuously producing the vulcanization accelerator CBS comprises a continuous reaction device consisting of a first reaction chamber, a second reaction chamber, a third reaction chamber and a fourth reaction chamber, wherein the upper part of the first reaction chamber is provided with an opening communicated with the second reaction chamber; the lower part of the second reaction chamber is provided with an opening communicated with the third reaction chamber; the upper part of the third reaction chamber is provided with an opening communicated with the fourth reaction chamber; the upper part of the fourth reaction chamber is provided with a discharge hole;
the M slurry metering pump and the cyclohexylamine metering pump are respectively communicated with the first reaction chamber through pipelines, and the hydrogen peroxide metering pump is respectively communicated with the first reaction chamber, the second reaction chamber and the third reaction chamber through three pipelines; the sodium hypochlorite metering pump is communicated with the fourth reaction chamber through a pipeline;
an M slurry flow regulating valve group is arranged on a pipeline between the M slurry metering pump and the first reaction chamber;
a cyclohexylamine flow regulating valve group is arranged on a pipeline between the cyclohexylamine metering pump and the first reaction chamber;
a first hydrogen peroxide flow regulating valve group is arranged on a pipeline between the hydrogen peroxide metering pump and the first reaction chamber;
a second hydrogen peroxide flow regulating valve group is arranged on a pipeline between the hydrogen peroxide metering pump and the second reaction chamber;
a third hydrogen peroxide flow regulating valve group is arranged on a pipeline between the hydrogen peroxide metering pump and the third reaction chamber;
a sodium hypochlorite flow regulating valve group is arranged on a pipeline between the sodium hypochlorite metering pump and the fourth reaction chamber;
the inlet end of the M slurry metering pump is communicated with the continuous mixing device;
the accelerator M bin and the water metering pump are respectively communicated with the continuous mixing device through pipelines.
In the device, the continuous reaction device comprises four reaction chambers, the outlet of the first reaction chamber is arranged at the upper part, the outlet of the second reaction chamber is arranged at the lower part, the outlet of the third reaction chamber is arranged at the upper part, and the whole material can flow from the first reaction chamber to the fourth reaction chamber in a wave manner.
The balance of discharging and feeding of each reaction chamber can be kept through each flow regulating valve group, and continuous production is realized.
The device can be used for continuously producing the vulcanization accelerator CBS, can realize automatic control, has more stable product quality and avoids frequent operation process of intermittent production.
As a preferred scheme, an automatic metering discharging device is arranged at an outlet of the accelerator M bin. Through automatic measurement discharging device, automatic discharging, automatic measurement realize the automated production of whole process. The discharge amount of the accelerator M in the accelerator M bin can be controlled by a material level control system.
As preferred scheme, still be equipped with the feed bin on the promoter M feed bin and prevent bridging device.
As the preferred scheme, set up dust pelletizing system on the promoter M feed bin.
Preferably, the first reaction chamber, the second reaction chamber and the third reaction chamber are respectively provided with a hydrogen peroxide distributor; a sodium hypochlorite distributor is arranged in the fourth reaction chamber.
Set up hydrogen peroxide solution distributor and sodium hypochlorite distributor, be similar to the automatic even dropwise add of hydrogen peroxide solution and sodium hypochlorite, avoid local excessive.
Further, the hydrogen peroxide distributor and the sodium hypochlorite distributor are one of a tubular distributor, a nozzle distributor and a shower distributor.
Preferably, the end of the pipeline between the M slurry metering pump and the first reaction chamber is arranged at the lower part of the first reaction chamber; the tail end of a pipeline between the cyclohexylamine metering pump and the first reaction chamber is also arranged at the lower part of the first reaction chamber; the tail end of a pipeline between the hydrogen peroxide metering pump and the first reaction chamber is arranged in the middle of the first reaction chamber; the tail end of a pipeline between the hydrogen peroxide metering pump and the second reaction chamber is arranged at the upper part of the second reaction chamber; the tail end of a pipeline between the hydrogen peroxide metering pump and the third reaction chamber is arranged at the lower part of the third reaction chamber; the tail end of a pipeline between the sodium hypochlorite metering pump and the fourth reaction chamber is arranged at the lower part of the fourth reaction chamber. The tail end positions of the hydrogen peroxide and sodium hypochlorite pipelines are arranged relative to the opening positions of the corresponding reaction chambers.
As a preferable scheme, the first reaction chamber, the second reaction chamber, the third reaction chamber and the fourth reaction chamber are respectively provided with an independent stirring device; the first reaction chamber, the second reaction chamber, the third reaction chamber and the fourth reaction chamber are all jacket heating type reaction chambers. A stirring device is arranged, so that the reaction system is more uniform; jacket heating provides the necessary temperature for the reaction and is relatively uniform.
The method for continuously producing the vulcanization accelerator CBS by adopting the equipment comprises the following steps:
1) enabling an accelerator M to enter a continuous mixing device from an accelerator M bin, and enabling water to enter the continuous mixing device through a water metering pump; uniformly mixing an accelerant M and water in a continuous mixing device to form M slurry;
2) conveying the M slurry to a first reaction chamber, adding a certain amount of cyclohexylamine into the first reaction chamber, pumping hydrogen peroxide into the first reaction chamber, a second reaction chamber and a third reaction chamber, and pumping sodium hypochlorite into a fourth reaction chamber;
the M slurry flow regulating valve group and the cyclohexylamine flow regulating valve group regulate the volume ratio of the M slurry to the cyclohexylamine; the flow of hydrogen peroxide in the first reaction chamber is regulated by a first hydrogen peroxide flow regulating valve group, the flow of hydrogen peroxide in the second reaction chamber is regulated by a second hydrogen peroxide flow regulating valve group, and the flow of hydrogen peroxide in the third reaction chamber is regulated by a third hydrogen peroxide flow regulating valve group; the flow of the sodium hypochlorite is regulated by a sodium hypochlorite flow regulating valve group;
3) and (3) feeding the reacted materials into a water washing device from a discharge hole on the fourth reaction chamber, washing the materials with water, dehydrating and drying to obtain a finished product of the vulcanization accelerator CBS.
As a preferred scheme, the reaction temperature in the first reaction chamber, the second reaction chamber, the third reaction chamber and the fourth reaction chamber is 30-60 ℃, and the retention time of materials in the continuous reaction device is 30-60 min.
Preferably, the mass ratio of the accelerator M to the water is 1: 1-2; the flow rate of the M slurry is 20-40 Kg/min, and the flow rate of the cyclohexylamine is 12-250 Kg/min; the flow of hydrogen peroxide in the first reaction chamber, the second reaction chamber and the third reaction chamber is 5-7 Kg/min; the flow rate of the sodium hypochlorite is 3.5-8 Kg/min.
As a preferred scheme, the mass fraction of the hydrogen peroxide is 12-20%; the sodium hypochlorite solution is 15-17% in effective content.
The invention has the beneficial effects that:
1. the production process is continuous, and quality fluctuation caused by difference between operation and equipment in the intermittent production process is avoided.
2. The reaction time is shortened, the production efficiency is improved, and the product production can be automated.
3. The reaction equipment has no blocking risk, the accelerant M can enter the reaction equipment in a slurry form, and the accelerant M does not need to be dissolved in cyclohexylamine or prepared into a salt solution, so that the product yield is ensured, and the salt content is not increased.
4. The invention has simple operation, high safety performance and good industrial application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic view of the structure of an apparatus for continuously producing a vulcanization accelerator CBS according to the present invention.
Detailed Description
Example 1
Equipment for continuously producing vulcanization accelerator CBS
As shown in figure 1, the equipment for continuously producing the vulcanization accelerator CBS comprises an accelerator M stock bin 1, a water metering pump 4, a continuous mixing device 2, a continuous reaction device 3, an M slurry metering pump 5, a cyclohexylamine metering pump 6, a hydrogen peroxide metering pump 7 and a sodium hypochlorite metering pump 8.
The continuous reaction device 3 is composed of a first reaction chamber 3-1, a second reaction chamber 3-2, a third reaction chamber 3-3 and a fourth reaction chamber 3-4.
The upper part of the first reaction chamber 3-1 is provided with a first opening 3-5 communicated with the second reaction chamber 3-2; the lower part of the second reaction chamber 3-2 is provided with a second opening 3-6 communicated with the third reaction chamber 3-3; the upper part of the third reaction chamber 3-3 is provided with a third opening 3-7 communicated with the fourth reaction chamber 3-4; the upper part of the fourth reaction chamber 3-4 is provided with a discharge hole 3-8. In the apparatus of the present invention, the continuous reaction device comprises four reaction chambers, the outlet of the first reaction chamber 3-1 is at the upper part, the outlet of the second reaction chamber 3-2 is at the lower part, the outlet of the third reaction chamber 3-3 is at the upper part, and the whole material flows from the first reaction chamber 3-1 to the fourth reaction chamber 3-4 in a wave-like manner.
The first reaction chamber 3-1, the second reaction chamber 3-2, the third reaction chamber 3-3 and the fourth reaction chamber 3-4 are all provided with independent stirring devices. The first reaction chamber 3-1, the second reaction chamber 3-2, the third reaction chamber 3-3 and the fourth reaction chamber 3-4 are all jacket heating type reaction chambers; jacket heating provided the necessary temperature for the reaction.
The accelerator M bin 1 is provided with an automatic metering and discharging device 1-3, and the side surface of the accelerator M bin 1 is provided with a bin bridge-preventing device 1-2. In some preferred embodiments, a dust removal system 1-1 can also be arranged on the bin 1 of the accelerator M.
The accelerator M bin 1 is communicated to the continuous mixing device 2 through a pipeline, and meanwhile, the water metering pump 4 is also communicated to the continuous mixing device 2 through a pipeline; water and accelerator M may be mixed together in a continuous mixing device 2 to form a slurry of M.
The continuous mixing device 2 is communicated to the first reaction chamber 3-1 through a pipeline, and an M slurry metering pump 5 and an M slurry flow regulating valve group 12 are respectively arranged on the pipeline between the continuous mixing device 2 and the first reaction chamber 3-1. The end of the pipeline between the continuous mixing device 2 and the first reaction chamber 3-1 is arranged at the lower part of the first reaction chamber 3-1.
An inlet of the cyclohexylamine metering pump 6 is communicated with a cyclohexylamine storage tank (not shown in the figure) through a pipeline, an outlet of the cyclohexylamine metering pump 6 is communicated to the first reaction chamber 3-1 through a pipeline, and a cyclohexylamine quantity regulating valve group 11 is arranged on the pipeline between the cyclohexylamine metering pump 6 and the first reaction chamber 3-1. The end of the line between the cyclohexylamine metering pump 6 and the first reaction chamber 3-1 is also disposed at the lower portion of the first reaction chamber 3-1.
The hydrogen peroxide metering pump 7 is respectively communicated to a first hydrogen peroxide distributor 310 in the first reaction chamber 3-1, a second hydrogen peroxide distributor 311 in the second reaction chamber 3-2 and a third hydrogen peroxide distributor 312 in the third reaction chamber 3-3 through three pipelines; a first hydrogen peroxide flow regulating valve group 13 is arranged on a pipeline between the hydrogen peroxide metering pump 7 and the first reaction chamber 3-1; a second hydrogen peroxide flow regulating valve group 14 is arranged on a pipeline between the hydrogen peroxide metering pump 7 and the second reaction chamber 3-2; a third hydrogen peroxide flow regulating valve group 10 is arranged on a pipeline between the hydrogen peroxide metering pump 7 and the third reaction chamber 3-3.
The tail end of a pipeline between the hydrogen peroxide metering pump 7 and the first reaction chamber 3-1 is arranged in the middle of the first reaction chamber 3-1; the tail end of a pipeline between the hydrogen peroxide metering pump 7 and the second reaction chamber 3-2 is arranged at the upper part of the second reaction chamber 3-2; the tail end of a pipeline between the hydrogen peroxide metering pump 7 and the third reaction chamber 3-3 is arranged at the lower part of the third reaction chamber 3-3;
the sodium hypochlorite metering pump 8 is communicated with a sodium hypochlorite distributor 313 in the fourth reaction chamber 3-4 through a pipeline; a sodium hypochlorite flow regulating valve group 9 is arranged on a pipeline between the sodium hypochlorite metering pump 8 and the fourth reaction chamber 3-4. The end of the pipeline between the sodium hypochlorite metering pump 8 and the fourth reaction chamber 3-4 is arranged at the lower part of the fourth reaction chamber 3-4.
The first hydrogen peroxide distributor 310, the second hydrogen peroxide distributor 311, the third hydrogen peroxide distributor 312 and the sodium hypochlorite distributor 313 may be one of a pipe distributor, a nozzle distributor and a shower distributor, and are preferably pipe distributors. The first hydrogen peroxide distributor 310, the second hydrogen peroxide distributor 311, the third hydrogen peroxide distributor 312 and the sodium hypochlorite distributor 313 are arranged to be similar to automatic uniform dripping of hydrogen peroxide and sodium hypochlorite, so that local excessive water is avoided.
The balance of discharging and feeding of each reaction chamber can be kept through each flow regulating valve group, and continuous production is realized.
The device can be used for continuously producing the vulcanization accelerator CBS, can realize automatic control, has more stable product quality and avoids frequent operation process of intermittent production.
Example 2
A method for continuously producing the vulcanization accelerator CBS using the apparatus in example 1, comprising the steps of:
1) enabling an accelerator M to enter a continuous mixing device from an accelerator M bin, and enabling water to enter the continuous mixing device through a water metering pump; uniformly mixing an accelerant M and water in a mass ratio of 1:1 in a continuous mixing device to form M slurry;
2) conveying the M slurry to a first reaction chamber 3-1, adding a certain amount of cyclohexylamine into the first reaction chamber 3-1, pumping hydrogen peroxide into the first reaction chamber 3-1, a second reaction chamber 3-2 and a third reaction chamber 3-3, and pumping sodium hypochlorite into a fourth reaction chamber 3-4;
the volume ratio of the M slurry to the cyclohexylamine is adjusted by an M slurry flow adjusting valve group 12 and a cyclohexylamine flow adjusting valve group 11; the flow of hydrogen peroxide in the first reaction chamber 3-1 is regulated by a first hydrogen peroxide flow regulating valve group 13, the flow of hydrogen peroxide in the second reaction chamber 3-2 is regulated by a second hydrogen peroxide flow regulating valve group 14, and the flow of hydrogen peroxide in the third reaction chamber 3-3 is regulated by a third hydrogen peroxide flow regulating valve group 10; the flow of sodium hypochlorite is regulated by a sodium hypochlorite flow regulating valve group 9;
3) the reacted materials enter a water washing device (not shown in the figure) from a discharge port 3-8 on the fourth reaction chamber 3-4, and the materials are washed by water, dehydrated and dried to obtain a finished product of the vulcanization accelerator CBS.
Wherein the content of the first and second substances,
m slurry is pumped into a first reaction chamber 3-1 of the continuous reaction equipment at a flow rate of 20Kg/min, and 12.5Kg/min cyclohexylamine is pumped into the first reaction chamber 3-1.
5.2Kg/min of 12 percent hydrogen peroxide is pumped into the first reaction chamber 3-1, the second reaction chamber 3-2 and the third reaction chamber 3-3 respectively.
3.7Kg/min of sodium hypochlorite solution with effective chlorine content of 15-17% is pumped into the fourth reaction chamber 3-4.
The reaction temperature is controlled at 35 ℃, the retention time of the materials in the reaction equipment is 60min, the product yield is 98.5 percent and the initial melting point is 99.5 ℃ after the materials are washed and dried.
Example 3
A method for continuously producing the vulcanization accelerator CBS using the apparatus in example 1, comprising the steps of:
1) enabling an accelerator M to enter a continuous mixing device from an accelerator M bin, and enabling water to enter the continuous mixing device through a water metering pump; uniformly mixing an accelerant M and water in a mass ratio of 1:1 in a continuous mixing device to form M slurry;
2) conveying the M slurry to a first reaction chamber 3-1, adding a certain amount of cyclohexylamine into the first reaction chamber 3-1, pumping hydrogen peroxide into the first reaction chamber 3-1, a second reaction chamber 3-2 and a third reaction chamber 3-3, and pumping sodium hypochlorite into a fourth reaction chamber 3-4;
the volume ratio of the M slurry to the cyclohexylamine is adjusted by an M slurry flow adjusting valve group 12 and a cyclohexylamine flow adjusting valve group 11; the flow of hydrogen peroxide in the first reaction chamber 3-1 is regulated by a first hydrogen peroxide flow regulating valve group 13, the flow of hydrogen peroxide in the second reaction chamber 3-2 is regulated by a second hydrogen peroxide flow regulating valve group 14, and the flow of hydrogen peroxide in the third reaction chamber 3-3 is regulated by a third hydrogen peroxide flow regulating valve group 10; the flow of sodium hypochlorite is regulated by a sodium hypochlorite flow regulating valve group 9;
3) the reacted materials enter a water washing device (not shown in the figure) from a discharge port 3-8 on the fourth reaction chamber 3-4, and the materials are washed by water, dehydrated and dried to obtain a finished product of the vulcanization accelerator CBS.
Wherein the content of the first and second substances,
m slurry was pumped into the first reaction chamber 3-1 of the continuous reaction apparatus at a flow rate of 27Kg/min, while 20Kg/min cyclohexylamine was pumped into the first reaction chamber 3-1.
5.5Kg/min of 15% hydrogen peroxide is pumped into the first reaction chamber 3-1, the second reaction chamber 3-2 and the third reaction chamber 3-3 respectively.
5Kg/min of sodium hypochlorite solution with effective chlorine content of 15-17% is pumped into the fourth reaction chamber 3-4.
The reaction temperature is controlled at 40 ℃, the retention time of the materials in the reaction equipment is 45min, the product yield is 98.0 percent and the initial melting point is 99.2 ℃ after the materials are washed and dried.
Example 4
A method for continuously producing the vulcanization accelerator CBS using the apparatus in example 1, comprising the steps of:
1) enabling an accelerator M to enter a continuous mixing device from an accelerator M bin, and enabling water to enter the continuous mixing device through a water metering pump; uniformly mixing an accelerant M and water in a mass ratio of 1:1 in a continuous mixing device to form M slurry;
2) conveying the M slurry to a first reaction chamber 3-1, adding a certain amount of cyclohexylamine into the first reaction chamber 3-1, pumping hydrogen peroxide into the first reaction chamber 3-1, a second reaction chamber 3-2 and a third reaction chamber 3-3, and pumping sodium hypochlorite into a fourth reaction chamber 3-4;
the volume ratio of the M slurry to the cyclohexylamine is adjusted by an M slurry flow adjusting valve group 12 and a cyclohexylamine flow adjusting valve group 11; the flow of hydrogen peroxide in the first reaction chamber 3-1 is regulated by a first hydrogen peroxide flow regulating valve group 13, the flow of hydrogen peroxide in the second reaction chamber 3-2 is regulated by a second hydrogen peroxide flow regulating valve group 14, and the flow of hydrogen peroxide in the third reaction chamber 3-3 is regulated by a third hydrogen peroxide flow regulating valve group 10; the flow of sodium hypochlorite is regulated by a sodium hypochlorite flow regulating valve group 9;
3) the reacted materials enter a water washing device (not shown in the figure) from a discharge port 3-8 on the fourth reaction chamber 3-4, and the materials are washed by water, dehydrated and dried to obtain a finished product of the vulcanization accelerator CBS.
Wherein the content of the first and second substances,
m slurry was pumped into the first reaction chamber 3-1 of the continuous reaction apparatus at a flow rate of 40Kg/min, while 25Kg/min cyclohexylamine was pumped into the first reaction chamber 3-1.
Hydrogen peroxide with the concentration of 20 percent and 6.2Kg/min is pumped into the first reaction chamber 3-1, the second reaction chamber 3-2 and the third reaction chamber 3-3 respectively.
7.5 Kg/min of sodium hypochlorite solution with effective chlorine content of 15-17% is pumped into the fourth reaction chamber 3-4.
The reaction temperature is controlled at 45 ℃, the retention time of the materials in the reaction equipment is 30min, the product yield is 97.2 percent and the initial melting point is 99.0 ℃ after the materials are washed and dried.
The present invention is illustrated by the above embodiments, but the present invention is not limited to the above embodiments, and any modification or variation based on the present invention is within the scope of the claims.
Claims (10)
1. An apparatus for continuously producing a vulcanization accelerator CBS, characterized in that: the continuous reaction device comprises a continuous reaction device consisting of a first reaction chamber, a second reaction chamber, a third reaction chamber and a fourth reaction chamber, wherein the upper part of the first reaction chamber is provided with an opening communicated with the second reaction chamber; the lower part of the second reaction chamber is provided with an opening communicated with the third reaction chamber; the upper part of the third reaction chamber is provided with an opening communicated with the fourth reaction chamber; the upper part of the fourth reaction chamber is provided with a discharge hole;
the M slurry metering pump and the cyclohexylamine metering pump are respectively communicated with the first reaction chamber through pipelines, and the hydrogen peroxide metering pump is respectively communicated with the first reaction chamber, the second reaction chamber and the third reaction chamber through three pipelines; the sodium hypochlorite metering pump is communicated with the fourth reaction chamber through a pipeline;
an M slurry flow regulating valve group is arranged on a pipeline between the M slurry metering pump and the first reaction chamber;
a cyclohexylamine flow regulating valve group is arranged on a pipeline between the cyclohexylamine metering pump and the first reaction chamber;
a first hydrogen peroxide flow regulating valve group is arranged on a pipeline between the hydrogen peroxide metering pump and the first reaction chamber;
a second hydrogen peroxide flow regulating valve group is arranged on a pipeline between the hydrogen peroxide metering pump and the second reaction chamber;
a third hydrogen peroxide flow regulating valve group is arranged on a pipeline between the hydrogen peroxide metering pump and the third reaction chamber;
a sodium hypochlorite flow regulating valve group is arranged on a pipeline between the sodium hypochlorite metering pump and the fourth reaction chamber;
the inlet end of the M slurry metering pump is communicated with the continuous mixing device;
the accelerator M bin and the water metering pump are respectively communicated with the continuous mixing device through pipelines.
2. The apparatus for continuously producing a vulcanization accelerator CBS according to claim 1, wherein: and an automatic metering and discharging device is arranged at an outlet of the accelerator M bin.
3. The apparatus for continuously producing a vulcanization accelerator CBS according to claim 1 or 2, wherein: the first reaction chamber, the second reaction chamber and the third reaction chamber are respectively internally provided with a hydrogen peroxide distributor; a sodium hypochlorite distributor is arranged in the fourth reaction chamber.
4. The apparatus for continuously producing a vulcanization accelerator CBS according to claim 3, wherein: the hydrogen peroxide distributor and the sodium hypochlorite distributor are one of a tubular distributor, a nozzle distributor and a shower distributor.
5. The apparatus for continuously producing a vulcanization accelerator CBS according to claim 1, wherein: the tail end of a pipeline between the M slurry metering pump and the first reaction chamber is arranged at the lower part of the first reaction chamber; the tail end of a pipeline between the cyclohexylamine metering pump and the first reaction chamber is also arranged at the lower part of the first reaction chamber; the tail end of a pipeline between the hydrogen peroxide metering pump and the first reaction chamber is arranged in the middle of the first reaction chamber; the tail end of a pipeline between the hydrogen peroxide metering pump and the second reaction chamber is arranged at the upper part of the second reaction chamber; the tail end of a pipeline between the hydrogen peroxide metering pump and the third reaction chamber is arranged at the lower part of the third reaction chamber; the tail end of a pipeline between the sodium hypochlorite metering pump and the fourth reaction chamber is arranged at the lower part of the fourth reaction chamber.
6. The apparatus for continuously producing a vulcanization accelerator CBS according to claim 1, wherein: the first reaction chamber, the second reaction chamber, the third reaction chamber and the fourth reaction chamber are all provided with independent stirring devices; the first reaction chamber, the second reaction chamber, the third reaction chamber and the fourth reaction chamber are all jacket heating type reaction chambers.
7. A method for the continuous production of the vulcanization accelerator CBS using the apparatus of claim 1, characterized by comprising the steps of:
1) enabling an accelerator M to enter a continuous mixing device from an accelerator M bin, and enabling water to enter the continuous mixing device through a water metering pump; uniformly mixing an accelerant M and water in a continuous mixing device to form M slurry;
2) conveying the M slurry to a first reaction chamber, adding a certain amount of cyclohexylamine into the first reaction chamber, pumping hydrogen peroxide into the first reaction chamber, a second reaction chamber and a third reaction chamber, and pumping sodium hypochlorite into a fourth reaction chamber;
the M slurry flow regulating valve group and the cyclohexylamine flow regulating valve group regulate the volume ratio of the M slurry to the cyclohexylamine; the flow of hydrogen peroxide in the first reaction chamber is regulated by a first hydrogen peroxide flow regulating valve group, the flow of hydrogen peroxide in the second reaction chamber is regulated by a second hydrogen peroxide flow regulating valve group, and the flow of hydrogen peroxide in the third reaction chamber is regulated by a third hydrogen peroxide flow regulating valve group; the flow of the sodium hypochlorite is regulated by a sodium hypochlorite flow regulating valve group;
3) and (3) feeding the reacted materials into a water washing device from a discharge hole on the fourth reaction chamber, washing the materials with water, dehydrating and drying to obtain a finished product of the vulcanization accelerator CBS.
8. The process for the continuous production of the vulcanization accelerator CBS as claimed in claim 7, wherein: the reaction temperature in the first reaction chamber, the second reaction chamber, the third reaction chamber and the fourth reaction chamber is 30-60 ℃, and the residence time of materials in the continuous reaction device is 30-60 min.
9. The process for the continuous production of the vulcanization accelerator CBS according to claim 7 or 8, wherein: the mass ratio of the accelerator M to the water is 1: 1-2; the flow rate of the M slurry is 20-40 kg/min, and the flow rate of the cyclohexylamine is 12-250 kg/min; the flow of hydrogen peroxide in the first reaction chamber, the second reaction chamber and the third reaction chamber is 5-7 kg/min; the flow rate of the sodium hypochlorite is 3.5-8 kg/min.
10. The process for the continuous production of the vulcanization accelerator CBS according to claim 7 or 8, wherein: the mass fraction of the hydrogen peroxide is 12-20%; the sodium hypochlorite solution is a sodium hypochlorite solution with the effective chlorine content of 15-17%.
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