CN111909072A - Preparation process of cyclohexanone peroxide ointment - Google Patents
Preparation process of cyclohexanone peroxide ointment Download PDFInfo
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- CN111909072A CN111909072A CN202010872482.5A CN202010872482A CN111909072A CN 111909072 A CN111909072 A CN 111909072A CN 202010872482 A CN202010872482 A CN 202010872482A CN 111909072 A CN111909072 A CN 111909072A
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- Prior art keywords
- cyclohexanone
- cyclohexanone peroxide
- tank
- reaction kettle
- peroxide
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- UICXTANXZJJIBC-UHFFFAOYSA-N 1-(1-hydroperoxycyclohexyl)peroxycyclohexan-1-ol Chemical compound C1CCCCC1(O)OOC1(OO)CCCCC1 UICXTANXZJJIBC-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000002674 ointment Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 70
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 claims abstract description 64
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims abstract description 54
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 38
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229960001826 dimethylphthalate Drugs 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000007599 discharging Methods 0.000 claims abstract description 18
- 238000005086 pumping Methods 0.000 claims abstract description 15
- 238000003860 storage Methods 0.000 claims abstract description 15
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 239000000945 filler Substances 0.000 claims abstract description 12
- 239000011265 semifinished product Substances 0.000 claims abstract description 9
- 239000000047 product Substances 0.000 claims abstract description 7
- 239000012895 dilution Substances 0.000 claims abstract description 6
- 238000010790 dilution Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000007689 inspection Methods 0.000 claims abstract description 6
- 238000004806 packaging method and process Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- QFFVPLLCYGOFPU-UHFFFAOYSA-N barium chromate Chemical compound [Ba+2].[O-][Cr]([O-])(=O)=O QFFVPLLCYGOFPU-UHFFFAOYSA-N 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 239000003085 diluting agent Substances 0.000 claims description 3
- 229910021485 fumed silica Inorganic materials 0.000 claims description 3
- 230000005484 gravity Effects 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 6
- 230000001105 regulatory effect Effects 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000007726 management method Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation process of cyclohexanone peroxide ointment, which comprises the steps of pumping hydrogen peroxide and dilute sulfuric acid to a reaction kettle respectively, and introducing chilled water to a jacket of the reaction kettle; the method comprises the steps of pumping cyclohexanone and dimethyl phthalate into a high-level metering tank to prepare a mixed liquid, dropwise adding the mixed liquid into a reaction kettle, reacting cyclohexanone with hydrogen peroxide to generate cyclohexanone peroxide, cooling to room temperature after dropwise adding is finished, adding dimethyl phthalate for dilution to obtain cyclohexanone peroxide paste, vacuumizing the cyclohexanone peroxide paste to a material discharging tank, automatically flowing the cyclohexanone peroxide paste to a transfer tank for temporary storage from the material discharging tank, pumping a cyclohexanone peroxide semi-finished product into a dispersion pot by using a vacuum pump, adding a filler and a toner, producing a cyclohexanone peroxide factice finished product through dispersion grinding, and finally packaging after inspection.
Description
Technical Field
The invention particularly relates to a preparation process of cyclohexanone peroxide ointment.
Background
Cyclohexanone peroxide, white or light yellow needle crystal or powder, which is dissolved in alcohol, benzene, acetic acid, petroleum ether and acetone, is insoluble in water and has strong oxidizing property; mainly used as a cross-linking agent and an initiator for rubber and plastic synthesis.
The cyclohexanone peroxide ointment is one form of cyclohexanone peroxide, and the original cyclohexanone peroxide needs to be manually added into a reaction kettle by workers in the preparation process, and the production is carried out by manually controlling the reaction conditions, so that the production efficiency is low, the labor capacity of the workers is increased by the process, the production potential safety hazard is large, and the workers are easily injured.
Disclosure of Invention
In view of the above, the invention aims to provide a cyclohexanone peroxide ointment preparation process which can automatically control material addition and reaction treatment, improve the production efficiency of cyclohexanone peroxide ointment, reduce the labor capacity of workers and improve the production safety of the workers.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a preparation process of cyclohexanone peroxide ointment comprises the following steps:
step 1, preparing materials: preparing hydrogen peroxide, dilute sulfuric acid, cyclohexanone, dimethyl phthalate, a filler and toner according to the preparation of cyclohexanone peroxide ointment, wherein two parts of dimethyl phthalate are prepared;
step 2, the concrete steps of the raw material mixing reaction are as follows:
a. automatically pumping cyclohexanone and dimethyl phthalate from a storage tank to a high-level metering tank I through a vacuum pump to mix to prepare a mixed solution for later use;
b. hydrogen peroxide is automatically pumped into a high-level tank from a storage tank by a vacuum pump after the weight of the hydrogen peroxide is calculated by a flowmeter, weighed dilute sulfuric acid is pumped into a high-level metering tank II by vacuum, flows into a reaction kettle automatically under the gravity, and meanwhile, chilled water is introduced into a jacket of the reaction kettle, and the reaction kettle is cooled for standby before material mixing reaction;
c. dropwise adding a mixed solution prepared from cyclohexanone and dimethyl phthalate in a high-level metering tank I in the specific step a into a reaction kettle in a dropwise adding mode, reacting cyclohexanone in the mixed solution with hydrogen peroxide in the kettle to generate cyclohexanone peroxide, controlling the dropwise adding speed of the mixed solution of the cyclohexanone and the dimethyl phthalate by a temperature control automatic interlocking system to keep the temperature not more than 40 ℃ in the reaction process, continuously cooling to room temperature after the dropwise adding is finished, and adding the dimethyl phthalate for dilution to prepare cyclohexanone peroxide paste for later use;
and step 3: after diluting the prepared cyclohexanone peroxide paste in the specific step c in the step 2, opening a bottom valve of the reaction kettle under the control of a control room, vacuumizing the cyclohexanone peroxide paste to a discharging tank for storage, and guiding the cyclohexanone peroxide paste to a transfer tank for temporary storage in a self-flowing manner by a discharging tank of the discharging tank;
and 4, step 4: automatically starting a vacuum pump to pump the cyclohexanone peroxide semi-finished product temporarily stored in the transit tank into a dispersion pot, then adding filler and toner, and producing a cyclohexanone peroxide ointment finished product for later use by running and grinding the cyclohexanone peroxide semi-finished product through the dispersion pot;
and 5: and packaging after passing the inspection.
Further, the filler in the step 1 is a mixture of fumed silica and raw powder.
Further, the toner in the step 1 is permanent yellow.
Further, the solid content of the cyclohexanone peroxide ointment prepared in the specific step c in the step 1 is less than or equal to 72 percent, and the content of the diluent dimethyl phthalate is more than or equal to 28 percent.
The technical effects of the invention are mainly reflected in the following aspects: pumping hydrogen peroxide and dilute sulfuric acid to a reaction kettle respectively, and introducing chilled water to a jacket of the reaction kettle simultaneously; the method comprises the steps of pumping cyclohexanone and dimethyl phthalate into a high-level metering tank to prepare a mixed liquid, dropwise adding the mixed liquid into a reaction kettle, reacting cyclohexanone with hydrogen peroxide to generate cyclohexanone peroxide, cooling to room temperature after dropwise adding is finished, adding dimethyl phthalate for dilution to obtain cyclohexanone peroxide paste, vacuumizing the cyclohexanone peroxide paste to a material discharging tank, automatically flowing the cyclohexanone peroxide paste to a transfer tank for temporary storage from the material discharging tank, pumping a cyclohexanone peroxide semi-finished product into a dispersion pot by using a vacuum pump, adding a filler and a toner, producing a cyclohexanone peroxide factice finished product through dispersion grinding, and finally packaging after inspection.
Detailed Description
The embodiments of the present invention are described in further detail to make the technical solutions of the present invention easier to understand and master.
Examples
A preparation process of cyclohexanone peroxide ointment comprises the following steps:
step 1, preparing materials: preparing hydrogen peroxide, dilute sulfuric acid, cyclohexanone, dimethyl phthalate, a filler and toner according to the preparation of cyclohexanone peroxide ointment, wherein two parts of dimethyl phthalate are prepared;
step 2, the concrete steps of the raw material mixing reaction are as follows:
a. automatically pumping cyclohexanone and dimethyl phthalate from a storage tank to a high-level metering tank I through a vacuum pump to mix to prepare a mixed solution for later use;
b. hydrogen peroxide is automatically pumped into a high-level tank from a storage tank by a vacuum pump after the weight of the hydrogen peroxide is calculated by a flowmeter, weighed dilute sulfuric acid is pumped into a high-level metering tank II by vacuum, flows into a reaction kettle automatically under the gravity, and meanwhile, chilled water is introduced into a jacket of the reaction kettle, and the reaction kettle is cooled for standby before material mixing reaction;
c. dropwise adding a mixed solution prepared from cyclohexanone and dimethyl phthalate in a high-level metering tank I in the specific step a into a reaction kettle in a dropwise adding mode, reacting cyclohexanone in the mixed solution with hydrogen peroxide in the kettle to generate cyclohexanone peroxide, controlling the dropwise adding speed of the mixed solution of the cyclohexanone and the dimethyl phthalate by a temperature control automatic interlocking system to keep the temperature not more than 40 ℃ in the reaction process, continuously cooling to room temperature after the dropwise adding is finished, and adding the dimethyl phthalate for dilution to prepare cyclohexanone peroxide paste for later use;
and step 3: after diluting the prepared cyclohexanone peroxide paste in the specific step c in the step 2, opening a bottom valve of the reaction kettle under the control of a control room, vacuumizing the cyclohexanone peroxide paste to a discharging tank for storage, and guiding the cyclohexanone peroxide paste to a transfer tank for temporary storage in a self-flowing manner by a discharging tank of the discharging tank;
and 4, step 4: automatically starting a vacuum pump to pump the cyclohexanone peroxide semi-finished product temporarily stored in the transit tank into a dispersion pot, then adding filler and toner, and producing a cyclohexanone peroxide ointment finished product for later use by running and grinding the cyclohexanone peroxide semi-finished product through the dispersion pot;
and 5: and packaging after passing the inspection.
In this embodiment, the filler in step 1 is a mixture of fumed silica and green powder.
In this embodiment, the toner in step 1 is permanent yellow.
In this example, the solid content of the cyclohexanone peroxide ointment prepared in the specific step c in step 1 is not more than 72%, and the content of the diluent dimethyl phthalate is not less than 28%.
In this example, the cyclohexanone peroxide ointment production process automation control measures:
first, control system principle:
the control mode of a PLC control system is adopted, a temperature transmitter and a pressure transmitter are arranged on the reaction kettle to detect temperature and pressure, when the set high limit is reached, sound and light alarm is given, an emergency cooling program is automatically started, cooling operation is carried out on the reaction kettle, and a raw material feeding cut-off valve is closed.
Secondly, description of a control system:
proportionally adding the measured production raw materials of hydrogen peroxide and dilute sulfuric acid into a reaction kettle according to process control indexes for mixing, pumping cyclohexanone and dimethyl phthalate into a high-level metering tank for mixing, and dropwise adding the mixture into the reaction kettle through a pipeline, wherein a dropwise adding pipeline of the high-level metering tank I is provided with an electromagnetic valve and an adjusting valve, a cooling water pipeline is arranged on the reaction kettle and is directly communicated with the reaction kettle, and a normally closed electromagnetic valve is arranged on the cooling water pipeline; in the reaction process, a cold water pump is started to use jacket low-temperature water for uninterrupted cooling, a PLC control system is used for opening an electromagnetic valve and an adjusting valve on a dropping pipeline, and the dropping speed of the materials is adjusted by controlling the opening of the adjusting valve, so that the temperature of the materials in the pot is stabilized below 40 ℃.
The reaction temperature must be controlled not to exceed 40 ℃ in the dripping process, when the temperature is higher than 40 ℃, the PLC temperature control automatic interlocking system closes the regulating valve and the stop valve on the dripping pipeline, the feeding is stopped, and simultaneously, the jacket low-temperature water is used for cooling the reaction kettle uninterruptedly; when the temperature is higher than 44 ℃, the alarm gives an alarm automatically, a pneumatic valve of a cooling water pipeline on the reaction kettle is opened through the PLC control system, and cooling water is injected into the reaction kettle to dilute and cool.
Thirdly, control system accident situation:
under the condition of system failure or power failure, the PLC system can automatically start a standby power supply, and a stop valve and an adjusting valve on the dripping pipeline can be automatically closed to stop dripping; when the PLC system interlocking device fails, a post operator can close a manual valve on the dripping pipeline to stop feeding; when the PLC system interlocking device is in a failure accident state, the materials in the reaction kettle are discharged into an accident receiving groove; in addition, in the production process, the management of operators is strengthened, the operators are forbidden to leave the post, the feeding accuracy is improved, and stainless steel or plastic tools are needed for containing products.
In this example, the operation mode of each apparatus in the cyclohexanone peroxide ointment production process:
the method comprises the following steps: quality field display is arranged, and interlocking control is carried out with a dimethyl phthalate delivery pump.
High-level jar: the liquid level display, the alarm and the flow display are arranged and are all linked with the vacuum pump and the tank area conveying pump, when the liquid level height reaches an alarm value during feeding (when feeding materials reach a certain quality), the feeding valve, the vacuum tube pneumatic valve, the pumping pipeline valve and the automatic stop conveying pump and the vacuum pump are automatically closed.
③ high-level metering tank: the liquid level display, the alarm and the flow display are arranged and are all linked with the vacuum pump and the tank area conveying pump, when the liquid level height reaches an alarm value during feeding, the feeding valve, the vacuum tube pneumatic valve, the pumping pipeline valve, the automatic stop conveying pump and the vacuum pump are automatically closed.
Pressure linkage and temperature linkage of chilled water circulation system
A chilled water inlet and outlet valve of a reaction kettle jacket is normally opened, a pressure transmitter is arranged on a circulating chilled water inlet pipeline, and when the pressure of the chilled water in the pipeline is reduced to be close to zero, a dropwise adding regulating valve and a pneumatic cutting ball valve of a high-level metering tank filled with mixed liquid of cyclohexanone and dimethyl phthalate are automatically closed; the freezing water tank is provided with a temperature transmitter and an on-site temperature display instrument, and when the temperature of the freezing water is higher than a set value of 20 ℃, a dropping regulating valve and a pneumatic cutting ball valve of a high-level metering tank filled with the mixed liquid of cyclohexanone and dimethyl phthalate are automatically closed; the freezing water tank is provided with a liquid level high-low alarm and is remotely transmitted to the control room. When the liquid level of the water tank is lower than a set value, the water replenishing valve is automatically opened to replenish water, and when the liquid level of the water tank is higher than the set value, the water replenishing valve is automatically closed.
Reaction temperature automatic control
The reaction kettle is provided with a temperature field display and a temperature transmitter, and is provided with automatic control and safety linkage of reaction temperature, when the temperature is 45 ℃, a high limit alarm is set, when the temperature is 50 ℃, a high limit alarm is set, a regulating valve and an emergency cut-off valve are arranged on a dripping pipeline of mixed liquid of cyclohexanone and dimethyl phthalate, the dripping flow of the mixed liquid of cyclohexanone is automatically regulated by using the reaction temperature, the reaction temperature is kept below 40 ℃, when the temperature in the kettle reaches 40 ℃, the regulating valve is automatically closed to stop dripping operation, and meanwhile, an emergency cut-off pneumatic ball valve is automatically closed; when the temperature of the materials in the reaction kettle is reduced to below 40 ℃, the emergency cut-off valve on the dripping pipe is opened again, and meanwhile, the cyclohexanone mixed solution is dripped through the regulating valve, so that the reaction temperature is kept below 40 ℃.
One of the safety chains of the reaction kettle: emergency water adding cooling to stop reaction
The reaction kettle is provided with an emergency water adding valve, when the temperature of materials in the reaction kettle exceeds 45 ℃, the high limit alarm is given, the alarm instrument whistles and automatically starts the interlocking protection system, the emergency water adding valve at the bottom of the water head tank at the upper part of the reaction kettle is automatically opened to add water into the reaction kettle for cooling, and the reaction is stopped.
Seventhly, the second safety chain of the reaction kettle: emergency emptying
When the temperature of the materials in the reaction kettle exceeds 50 ℃, the high limit alarms, the alarm whistles and automatically starts the interlocking protection system, an emergency water adding valve at the bottom of a water head tank at the upper part of the reaction kettle is automatically opened to add water into the reaction kettle for cooling, the reaction is stopped, an emergency emptying valve at the lower part of the reaction kettle is opened by a control room, and the materials in the reaction kettle are discharged into an emergency tank for accidents.
Eighthly, discharging a pump: and a pressure indicator is arranged on an outlet pipeline of the discharging pump, and the discharging pump automatically stops when the pressure is zero.
Ninthly, transferring the trough: the transfer tank is provided with a temperature transmitter and a field thermometer, is provided with a temperature high-level alarm and is remotely transmitted to a control room; when the temperature exceeds 45 ℃, the high-limit alarm is carried out, the alarm instrument sounds a whistle, an operator emergently opens an emergency discharge valve at the bottom, the materials are discharged into the accident receiving groove, meanwhile, water is added for cooling, and the decomposition reaction is stopped.
R dispersion boiler: the dispersion pot is provided with a temperature transmitter and a pressure transmitter, and is provided with a high-level alarm system which is remotely transmitted back to the control room, the vacuumizing is automatically stopped when the vacuum degree reaches-0.08 mpa, and the alarm buzzes when the temperature exceeds 40 ℃; when the temperature is raised to 50 ℃, the emergency water valve is automatically opened.
The technical effects of the invention are mainly reflected in the following aspects: pumping hydrogen peroxide and dilute sulfuric acid to a reaction kettle respectively, and introducing chilled water to a jacket of the reaction kettle simultaneously; the method comprises the steps of pumping cyclohexanone and dimethyl phthalate into a high-level metering tank to prepare a mixed liquid, dropwise adding the mixed liquid into a reaction kettle, reacting cyclohexanone with hydrogen peroxide to generate cyclohexanone peroxide, cooling to room temperature after dropwise adding is finished, adding dimethyl phthalate for dilution to obtain cyclohexanone peroxide paste, vacuumizing the cyclohexanone peroxide paste to a material discharging tank, automatically flowing the cyclohexanone peroxide paste to a transfer tank for temporary storage from the material discharging tank, pumping a cyclohexanone peroxide semi-finished product into a dispersion pot by using a vacuum pump, adding a filler and a toner, producing a cyclohexanone peroxide factice finished product through dispersion grinding, and finally packaging after inspection.
The above are only typical examples of the present invention, and besides, the present invention may have other embodiments, and all the technical solutions formed by equivalent substitutions or equivalent changes are within the scope of the present invention as claimed.
Claims (4)
1. A preparation process of cyclohexanone peroxide ointment is characterized by comprising the following steps:
step 1, preparing materials: preparing hydrogen peroxide, dilute sulfuric acid, cyclohexanone, dimethyl phthalate, a filler and toner according to the preparation of cyclohexanone peroxide ointment, wherein two parts of dimethyl phthalate are prepared;
step 2, the concrete steps of the raw material mixing reaction are as follows:
a. automatically pumping cyclohexanone and dimethyl phthalate from a storage tank to a high-level metering tank I through a vacuum pump to mix to prepare a mixed solution for later use;
b. hydrogen peroxide is automatically pumped into a high-level tank from a storage tank by a vacuum pump after the weight of the hydrogen peroxide is calculated by a flowmeter, weighed dilute sulfuric acid is pumped into a high-level metering tank II by vacuum, flows into a reaction kettle automatically under the gravity, and meanwhile, chilled water is introduced into a jacket of the reaction kettle, and the reaction kettle is cooled for standby before material mixing reaction;
c. dropwise adding a mixed solution prepared from cyclohexanone and dimethyl phthalate in a high-level metering tank I in the specific step a into a reaction kettle in a dropwise adding mode, reacting cyclohexanone in the mixed solution with hydrogen peroxide in the kettle to generate cyclohexanone peroxide, controlling the dropwise adding speed of the mixed solution of the cyclohexanone and the dimethyl phthalate by a temperature control automatic interlocking system to keep the temperature not more than 40 ℃ in the reaction process, continuously cooling to room temperature after the dropwise adding is finished, and adding the dimethyl phthalate for dilution to prepare cyclohexanone peroxide paste for later use;
and step 3: after diluting the prepared cyclohexanone peroxide paste in the specific step c in the step 2, opening a bottom valve of the reaction kettle under the control of a control room, vacuumizing the cyclohexanone peroxide paste to a discharging tank for storage, and guiding the cyclohexanone peroxide paste to a transfer tank for temporary storage in a self-flowing manner by a discharging tank of the discharging tank;
and 4, step 4: automatically starting a vacuum pump to pump the cyclohexanone peroxide semi-finished product temporarily stored in the transit tank into a dispersion pot, then adding filler and toner, and producing a cyclohexanone peroxide ointment finished product for later use by running and grinding the cyclohexanone peroxide semi-finished product through the dispersion pot;
and 5: and packaging after passing the inspection.
2. The process for preparing cyclohexanone peroxide ointment as claimed in claim 1, wherein: the filler in the step 1 is a mixture of fumed silica and raw powder.
3. The process for preparing cyclohexanone peroxide ointment as claimed in claim 1, wherein: the toner in the step 1 is permanent yellow.
4. The process for preparing cyclohexanone peroxide ointment as claimed in claim 1, wherein: the solid content of the cyclohexanone peroxide ointment prepared in the specific step c in the step 1 is less than or equal to 72 percent, and the content of the diluent dimethyl phthalate is more than or equal to 28 percent.
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| CN202010872482.5A CN111909072A (en) | 2020-08-26 | 2020-08-26 | Preparation process of cyclohexanone peroxide ointment |
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| CN202010872482.5A CN111909072A (en) | 2020-08-26 | 2020-08-26 | Preparation process of cyclohexanone peroxide ointment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116606562A (en) * | 2023-04-27 | 2023-08-18 | 英德市城泰化工有限公司 | Preparation method of high-dispersivity paste benzoyl peroxide for sheet metal ash |
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2020
- 2020-08-26 CN CN202010872482.5A patent/CN111909072A/en active Pending
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| CN107999011A (en) * | 2017-12-13 | 2018-05-08 | 方亨 | Methyl ethyl ketone peroxide production system and production technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116606562A (en) * | 2023-04-27 | 2023-08-18 | 英德市城泰化工有限公司 | Preparation method of high-dispersivity paste benzoyl peroxide for sheet metal ash |
| CN116606562B (en) * | 2023-04-27 | 2024-03-12 | 英德市城泰化工有限公司 | Preparation method of high-dispersivity paste benzoyl peroxide for sheet metal ash |
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Application publication date: 20201110 |
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| RJ01 | Rejection of invention patent application after publication |