CN203715541U - Production equipment for dicumyl peroxide condensation reaction - Google Patents
Production equipment for dicumyl peroxide condensation reaction Download PDFInfo
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- CN203715541U CN203715541U CN201320305036.1U CN201320305036U CN203715541U CN 203715541 U CN203715541 U CN 203715541U CN 201320305036 U CN201320305036 U CN 201320305036U CN 203715541 U CN203715541 U CN 203715541U
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Abstract
The utility model discloses production equipment for dicumyl peroxide condensation reaction. The production equipment comprises a condensation reaction kettle, wherein a preset amount of benzyl alcohol in a benzyl alcohol metering slot, a preset amount of catalyst and a preset amount of oxidization liquid in an oxidization liquid metering slot are sequentially fed into a condensation reaction kettle to carry out condensation reaction; during the condensation reaction, if a control system judges that conditions for starting primary temperature interconnected control are satisfied, a circulating hot water valve of the condensation reaction kettle is closed, and a circulating cooling water valve of the condensation reaction kettle is opened; if the control system judges that the conditions for starting secondary temperature interconnected control are satisfied, a condensation water-adding valve is opened, the circulating hot water valve of the condensation reaction kettle is closed, and the circulating cooling water valve of the condensation reaction kettle is opened. The primary temperature interconnected control and the secondary temperature interconnected control are adopted during the condensation reaction period, and therefore, the condensation reaction is ensured to safely and reliably produce according to processes.
Description
Technical field
The utility model relates to the production unit of dicumyl peroxide condensation reaction.
Background technology
Dicumyl peroxide is a kind of the most frequently used symmetrical dialkyl group organo-peroxide, the vulcanizing agent DCP that is otherwise known as, white crystals, 39 ℃～40 ℃ of fusing points, 120 ℃～125 ℃ of decomposition temperatures are stable under room temperature, see that light becomes micro-yellow gradually, theoretical active o content 5.92%.Dicumyl peroxide can be used as natural rubber, elastomeric vulcanizing agent, such as the vulcanizing agent as terpolymer EP rubber (EPDM), paracril and silicon rubber etc.Dicumyl peroxide also can be used as the initiator of polyreaction and the linking agent that is used as polyvinyl resin, for example, be typically used as the linking agent of polyethylene (PE), chlorinatedpolyethylene (CPE), polystyrene (PS).Dicumyl peroxide also can be used as the initiator of synthetic Expandable Polystyrene (EPS) (EPS), the whipping agent of plastic of poly vinyl acetate (EVA) etc.The molecular formula of dicumyl peroxide is C18H22O2, and chemical structure is as follows:
(formula 1)
After dicumyl peroxide is crosslinked, the physical properties of polymkeric substance is greatly improved, its heat impedance, chemical resistant properties, resistance to pressure, splitting resistance and physical strength all increase to some extent.Dicumyl peroxide can be widely used in the industries such as electric wire, shoemaking, building materials.
The principle of industrial production dicumyl peroxide is to take isopropyl benzene as raw material, by atmospheric oxidation, cumene oxidation is become to hydrogen phosphide cumene, and part hydrogen phosphide cumene is generated to α by reduction reaction, α-dimethyl benzyl alcohol (in this article its can referred to as benzylalcohol), then α, α-dimethyl benzyl alcohol and hydrogen phosphide cumene, under perchloric acid catalysis, carry out condensation reaction and generate dicumyl peroxide, and condensation reaction is final step reaction in dicumyl peroxide production, determining the quality of dicumyl peroxide.
The technique of the condensation reaction of the dicumyl peroxide of prior art (as shown in Equation 2) mainly comprises the following steps: under the effect of a small amount of perchloric acid catalysis agent, α, there is condensation reaction with hydrogen phosphide cumene (CHP) in α-dimethyl benzyl alcohol (CA), reaction obtains dicumyl peroxide condensated liquid at 42 ℃～45 ℃; Through alkali cleaning, washing, after processing, dicumyl peroxide condensated liquid is adjusted to neutrality; Then the concentrate that reduces pressure and recrystallization.
formula (2).
In the production process of dicumyl peroxide, adopt perchloric acid, as catalyzer, the condensation reaction of dicumyl peroxide is had to larger potential safety hazard.This is because perchloric acid is the strongest mineral acid, the condensation reaction of dicumyl peroxide is had to very strong katalysis, but dicumyl peroxide is also had to very strong sour Decomposition simultaneously, later stage of the condensation reaction of dicumyl peroxide particularly, when in system, benzylalcohol reduces in a large number, perchloric acid is the most violent to the decomposition of dicumyl peroxide, and this can cause violent exothermal decomposition reactions, when serious, can set off an explosion.
In the production process of dicumyl peroxide, because condensation reaction is strong exothermal reaction, for example, if the temperature of condensation reaction controls improper or charge ratio (proportioning of benzylalcohol and oxidation solution) is improper, likely can occurrence temperature control out of controlly, when serious, also can blast.
In the production process of dicumyl peroxide, for the production of feed intake benzylalcohol and the oxidation solution of the condensation reaction of dicumyl peroxide, there is strict input ratio requirement.And the benzylalcohol groove of prior art and oxidation liquid bath have only been installed on-the-spot liquidometer, make that the input distributing precision of benzylalcohol and oxidation solution is poor and error is large.If it is excessive that this drops into benzylalcohol, benzylalcohol consumption is large, the quality product of impact oxidation diisopropylbenzene(DIPB); If it is excessive that oxidation solution drops into, cause rising for the production of the temperature in the condensation reaction still of dicumyl peroxide too fast, temperature is controlled out of control, there is the risk of blasting.
In the production process of dicumyl peroxide, for the production of feeding intake in the condensation reaction still of dicumyl peroxide, must carry out according to the order of appointment, for example, if do not carry out (operator's mishandle) according to the order of appointment, may blast, the serious industrial accident such as spill-over.
In the production process of dicumyl peroxide, range of reaction temperature little (between 42-45 ℃) for the production of the condensation reaction still of dicumyl peroxide, and temperature of reaction control has certain hysteresis quality, this makes to work as something unexpected happened, as condensation reaction is not reacted, abnormal, the circulating water pressure fast-descending of oxidation solution content etc., makes temperature of reaction increase too fast uncontrollable, in the time of need adding in time water termination reaction, exist and find slowly, to add water not in time, the risk that very easily causes the accident or explode.
Therefore, must take measures to guarantee that the device security of producing the condensation reaction of oxidation diisopropylbenzene(DIPB) moves reliably,, expectation provides a kind of production unit and method that is oxidized diisopropylbenzene(DIPB) condensation reaction, so that guarantee that when improving the output of dicumyl peroxide and quality the production safety of dicumyl peroxide condensation reaction moves reliably.
Utility model content
The purpose of this utility model is to provide a kind of production unit of the condensation reaction for the production of dicumyl peroxide, to overcome the defect of prior art.
An embodiment of the present utility model provides a kind of production unit of dicumyl peroxide condensation reaction, and it comprises:
Condensation adds tank, accommodates for stopping the water of the predetermined amount of condensation reaction;
Benzylalcohol scale tank, accommodates the benzylalcohol for the predetermined amount of condensation reaction;
Oxidation solution scale tank, accommodates the oxidation solution for the predetermined amount of condensation reaction;
Condensation condenser, carries out condensation for the gaseous state isopropyl benzene to condensation reaction and water;
Catalyst feed pipeline, for joining condensation reaction still by the catalyzer of predetermined amount; And
Condensation reaction still, it adds tank with condensation respectively, benzylalcohol scale tank, oxidation solution scale tank and catalyst feed pipeline circulation connect, condensation adds tank and is connected with the circulation of condensation reaction still with the condensation priming valve being arranged on condensation filler pipe road by condensation filler pipe road, condensation reaction still is also connected with the circulation of condensation vacuum buffer tank by condensation condenser, condensation vacuum buffer tank is also connected with condensation vacuum pump, condensation vacuum pump is used for condensation condenser, condensation vacuum buffer tank and condensation reaction still vacuumize, in condensation reaction still, be also provided with condensation reaction still circulating cooling water coil and condensation reaction still agitator, condensation reaction still is also provided with condensation reaction still circulating hot water chuck outward, circulation is connected condensation reaction still circulating cooling water coil with condensation reaction still recirculated cooling water outlet valve with condensation reaction still circulating cooling water inlet valve, circulation is connected condensation reaction still circulating hot water chuck with condensation reaction still circulating hot water outlet valve with condensation reaction still circulating hot water inlet valve, the benzylalcohol of predetermined amount in benzylalcohol scale tank, the catalyzer of predetermined amount, in oxidation solution scale tank, the oxidation solution of predetermined amount is dosed into successively and in condensation reaction still, carries out condensation reaction, condensation reaction still circulating cooling water coil is used for making condensation reaction still recirculated cooling water to pass through wherein, condensation reaction still circulating hot water chuck is used for making condensation reaction still circulating hot water to pass through wherein,
Condensation top liquid bath, circulation is connected condensation top liquid bath with condensation condenser with condensation reaction still, after a part of gaseous state isopropyl benzene that condensation reaction produces and water condensation, directly collect in the liquid bath of condensation top, and another part gaseous state isopropyl benzene that condensation reaction produces and water are collected in the liquid bath of condensation top after by condensation condenser condenses; It is characterized in that, Controlling System, it is with temperature sensor in condensation reaction still, condensation reaction still agitator, be electrically connected to for the pressure transmitter of hydraulic pressure in sensing condensation filler pipe road, pressure transmitter, condensation priming valve, condensation reaction still circulating hot water inlet valve, condensation reaction still circulating cooling water inlet valve and condensation reaction still temperature interlocking emergency stop push button for hydraulic pressure in condensation reaction still circulating cooling water coil.
The production unit of the dicumyl peroxide condensation reaction providing according to above-mentioned embodiment of the present utility model, wherein
The production unit of dicumyl peroxide condensation reaction also comprises top fluid dewatering groove, and the condensed waste material of collecting in the liquid bath of condensation top is discharged in the fluid dewatering groove of top and carries out concentrate.
The production unit of the dicumyl peroxide condensation reaction providing according to above-mentioned embodiment of the present utility model, wherein the production unit of dicumyl peroxide condensation reaction also comprises the condensation washing kettle being connected with the bottom circulation of condensation reaction still, condensation washing kettle adds alkali scale tank, system vacuum pump, condensation lye vat with condensation, and circulation is connected with condensation alkali cleaning subsider, condensation alkali cleaning subsider is connected with the circulation of condensation lye vat and condensation water wash column respectively, and condensation water wash column and condensated liquid concentrated flow lead to and connect.
The production unit of the dicumyl peroxide condensation reaction providing according to above-mentioned embodiment of the present utility model; wherein the production unit of dicumyl peroxide condensation reaction also comprises condensation accident groove; in the situation that condensation reaction still is blasted; reaction solution in condensation reaction still can be filled in condensation accident groove, to protect condensation reaction on-the-spot.
The production unit of the dicumyl peroxide condensation reaction providing according to above-mentioned embodiment of the present utility model, wherein the production unit of dicumyl peroxide condensation reaction also comprises static mixer and the water-and-oil separator being successively set between condensation washing pump and condensation water wash column, wherein static mixer is used for making to wash hot water and mixes with condensated liquid, and water-and-oil separator is for to filtering the solid impurity of condensated liquid.
The production unit of the dicumyl peroxide condensation reaction providing according to above-mentioned embodiment of the present utility model, wherein benzylalcohol scale tank and benzylalcohol concentrated flow lead to and connect, for the benzylalcohol of the predetermined amount for condensation reaction of benzylalcohol groove is joined to benzylalcohol scale tank, oxidation solution scale tank and oxidation solution concentrated flow lead to and connect, for the oxidation solution of the predetermined amount for condensation reaction of oxidation liquid bath is joined to oxidation solution scale tank.
The production unit of the dicumyl peroxide condensation reaction providing according to above-mentioned embodiment of the present utility model, wherein benzylalcohol scale tank and oxidation solution scale tank include electrometer treasure separately, liquidometer and sampling valve, the electrometer treasure of benzylalcohol scale tank and liquidometer are for measuring the benzylalcohol of benzylalcohol scale tank, and the electrometer treasure of oxidation solution scale tank and liquidometer are for the oxidation solution metering to oxidation solution scale tank, the sampling valve of benzylalcohol scale tank samples and analyzes the weight percent content of benzylalcohol for the benzylalcohol to after metering, the sampling valve of oxidation solution scale tank samples and analyzes the weight percent content of oxidation solution for the oxidation solution to after metering.
According to the advantage of the production unit of dicumyl peroxide condensation reaction of the present utility model, be, owing to adopting firsts and seconds temperature interlocked control during condensation reaction, thereby guaranteed that condensation reaction produces safely and reliably by operation.
According to being also advantageous in that of the production unit of dicumyl peroxide condensation reaction of the present utility model, the waste material that to reduce people be mishandle, reclaimed condensation reaction has reduced material consumption, the utilization ratio that has improved hydrogen phosphide cumene, has improved quality product, improves product income.
Accompanying drawing explanation
Fig. 1 shows according to the production unit of dicumyl peroxide condensation reaction of the present utility model.
Fig. 2 shows according to the production method of dicumyl peroxide condensation reaction of the present utility model.
Parts and label list
| 1 | Benzylalcohol scale tank |
| 1a | Benzylalcohol groove |
| 1b | Benzylalcohol groove outlet valve |
| 1c | Benzylalcohol scale tank feed valve |
| 1d | Benzylalcohol scale tank reverse flow valve |
| 1e | Benzylalcohol scale tank vacuum valve |
| 1f | Benzylalcohol scale tank blow-off valve |
| 1g | Benzylalcohol scale tank hot water inlet valve |
| 1h | Benzylalcohol scale tank hot water outlet valve |
| 1j | Benzylalcohol scale tank sampling valve |
| 1l | Benzylalcohol feed valves |
| 2a | Oxidation liquid bath |
| 2b | Oxidation liquid bath outlet valve |
| 2c | Oxidation liquid bath reverse flow valve |
| 2d | Oxidation solution scale tank feed valve |
| 2e | Oxidation solution scale tank blow-off valve |
| 2f | Oxidation solution scale tank surplus valve |
| 2g | Oxidation solution feed valves |
| 2h | Oxidation liquid pump |
| 2l | Oxidation solution sampling valve |
| 2 | Oxidation solution scale tank |
| 3 | Condensation adds tank |
| 3a | Condensation adds tank feed valve |
| 3b | Condensation priming valve |
| 4 | Condensation reaction still |
| 4a | Condensation reaction still circulating cooling water coil |
| 4b | Condensation reaction still circulating hot water chuck |
| 4c | Condensation reaction still agitator |
| 4d | Condensation reaction still circulating hot water inlet valve |
| 4e | Condensation reaction still circulating hot water outlet valve |
| 4f | Condensation reaction still circulating cooling water inlet valve |
| 4g | Condensation reaction still recirculated cooling water outlet valve |
| 4h | Condensation reaction still sampling valve |
| 4j | Condensation reaction still bleeder valve |
| 41 | Condensation reaction still vacuum valve |
| 5 | Condensation accident groove |
| 5a | Rupture disk |
| 6 | Condensation condenser |
| 6a | Condensation condenser refrigerating fulid inlet valve |
| 6b | Condensation condenser refrigerating fulid outlet valve |
| 6c | Condensation condenser bleeder valve |
| 7 | Condensation washing kettle |
| 7a | Condensation washing kettle outlet valve |
| 7b | Condensation washing kettle blow-off valve |
| 7c | Condensation washing kettle condensation vacuum pump valve |
| 7d | Condensation washing kettle system vacuum pump valve |
| 7e | Condensation washing kettle agitator |
| 8 | Condensation vacuum buffer tank |
| 9 | Condensation adds alkali scale tank |
| 9a | Condensation alkali addition valve |
| 10 | Condensation alkali cleaning subsider |
| 10a | Condensation alkali cleaning subsider the first outlet valve |
| 10b | Condensation alkali cleaning subsider the second outlet valve |
| 10c | Condensation alkali cleaning subsider inlet valve |
| 11 | Condensation lye vat |
| 11a | Condensation lye vat blow-off valve |
| 11b | Condensation lye vat wastewater valve |
| 12 | Condensation water wash column |
| 12a | Condensation water wash column surplus valve |
| 12b | Condensation water wash column blow-off valve |
| 12c | Condensation water wash column wastewater valve |
| 12d | Condensation water wash column feed valve |
| 12e | Condensation water wash column the first hot water valve |
| 12f | Condensation water wash column the second hot water valve |
| 13 | Condensation liquid bath |
| 14 | Condensation liquid pump |
| 15 | Condensation washing pump |
| 16 | Static mixer |
| 17 | Water-and-oil separator |
| 18 | Condensation vacuum pump |
| 20 | Condensation top liquid bath |
| 20a | Condensation top liquid bath outlet valve |
| 20b | Top fluid dewatering groove feed valve |
| 21 | Bubbler valve |
| 22 | Bubbler |
| 24 | Catalyzer feed valves |
| 100 | Bian alcohol feeding pipeline |
| 101 | Oxidation solution feeding pipeline |
| 102 | Condensation filler pipe road |
| 103 | Condensation waste material pipeline |
| 104 | Condensation accident pipeline |
| 105 | Condensated liquid alkali cleaning pipeline |
| 106 | The second condenser pipe |
| 107 | The first condenser pipe |
| 108 | Condensation adds alkali pipeline |
| 109 | The second vacuum-lines |
| 110 | The first vacuum-lines |
| 111 | The 3rd vacuum-lines |
| 112 | The second recycle of alkali liquor road |
| 115 | Condensated liquid washing pipeline |
| 116 | Condensated liquid overflow passage |
| 117 | The second washing pipeline |
| 118 | The first washing pipeline |
| 120 | The first condensated liquid is collected pipeline |
| 121 | The first recycle of alkali liquor pipeline |
| 122 | Benzylalcohol metering pipeline |
| 123 | Oxidation solution metering pipeline |
| 124 | Oxidation solution the second return line |
| 125 | Oxidation solution the first return line |
| 126 | Benzylalcohol return line |
| 127 | Catalyzer feeding pipeline |
| 128 | The 4th vacuum-lines |
Embodiment
Fig. 1-2 and following declarative description optional embodiment of the present utility model with instruction those of ordinary skills, how to implement and to reproduce the utility model.In order to instruct technical solutions of the utility model, simplified or omitted some conventional aspects.It should be understood by one skilled in the art that and be derived from the modification of these embodiments or replace and will drop in protection domain of the present utility model.It should be understood by one skilled in the art that following characteristics can combine to form a plurality of modification of the present utility model in every way.Thus, the utility model is not limited to following optional embodiment, and only by claim and their equivalent, is limited.
Oxidation solution refers to the cumene solution of hydrogen phosphide cumene in this article, and α, α-dimethyl benzyl alcohol in this article also can be referred to as benzylalcohol.
An embodiment of the present utility model provides a kind of production unit (as shown in Figure 1) of dicumyl peroxide condensation reaction, and it comprises:
Condensation adds tank 3, accommodates for stopping the water of the predetermined amount of condensation reaction;
Benzylalcohol scale tank 1, accommodates the benzylalcohol for the predetermined amount of condensation reaction;
Oxidation solution scale tank 2, accommodates the oxidation solution for the predetermined amount of condensation reaction;
Condensation condenser 6, carries out condensation for the gaseous state isopropyl benzene to condensation reaction and water;
Catalyst feed pipeline 127, for joining condensation reaction still 4 by the catalyzer of predetermined amount;
Condensation reaction still 4, it adds tank 3 with condensation respectively, benzylalcohol scale tank 1, oxidation solution scale tank 2 and catalyst feed pipeline 127 circulations connect, condensation adds tank 3 and is connected with 4 circulations of condensation reaction still with the condensation priming valve 3b being arranged on condensation filler pipe road by condensation filler pipe road 102, condensation reaction still 4 is also connected with 8 circulations of condensation vacuum buffer tank by condensation condenser 6, condensation vacuum buffer tank 8 is also connected with condensation vacuum pump 18, condensation vacuum pump 18 is for to condensation condenser 6, condensation vacuum buffer tank 8 and condensation reaction still 4 vacuumize, in condensation reaction still 4, be also provided with condensation reaction still circulating cooling water coil 4a and condensation reaction still agitator 4c, the outer condensation reaction still circulating hot water chuck 4b that is also provided with of condensation reaction still 4, circulation is connected condensation reaction still circulating cooling water coil 4a with condensation reaction still recirculated cooling water outlet valve 4g with condensation reaction still circulating cooling water inlet valve 4f, circulation is connected condensation reaction still circulating hot water chuck 4b with condensation reaction still circulating hot water outlet valve 4e with condensation reaction still circulating hot water inlet valve 4d, the benzylalcohol of predetermined amount in benzylalcohol scale tank 1, the catalyzer of predetermined amount, in oxidation solution scale tank 2, the oxidation solution of predetermined amount is dosed into successively and in condensation reaction still 4, carries out condensation reaction, condensation reaction still circulating cooling water coil 4a is used for making condensation reaction still recirculated cooling water to pass through wherein, condensation reaction still circulating hot water chuck 4b is used for making condensation reaction still circulating hot water to pass through wherein, the flow of adjusting condensation reaction still recirculated cooling water and condensation reaction still circulating hot water is controlled the temperature of condensation reaction, when arriving condensation reaction terminal, the water that condensation is added to the predetermined amount in tank 3 joins in condensation reaction still and stops condensation reaction, wherein during feeding intake and before termination condensation reaction, all keep condensation reaction still agitator 4c in running condition,
Condensation top liquid bath 20,6 circulations are connected condensation top liquid bath 20 with condensation condenser with condensation reaction still 4, after a part of gaseous state isopropyl benzene that condensation reaction produces and water condensation, directly collect in condensation top liquid bath 20, and another part gaseous state isopropyl benzene that condensation reaction produces and water are collected in condensation top liquid bath 20 after by 6 condensations of condensation condenser; And
Controlling System, it is with temperature sensor in condensation reaction still, condensation reaction still agitator 4c, be electrically connected to for the pressure transmitter of hydraulic pressure in sensing condensation filler pipe road, pressure transmitter, condensation priming valve 3b, condensation reaction still circulating hot water inlet valve 4d, condensation reaction still circulating cooling water inlet valve 4f and condensation reaction still temperature interlocking emergency stop push button for hydraulic pressure in condensation reaction still circulating cooling water coil; wherein during condensation reaction, Controlling System is according to the signal that carrys out temperature sensor in self-condensation reaction still, the temperature of judging in condensation reaction still is not less than the first design temperature, start one-level temperature interlocked control, close condensation reaction still cycling hot water valve 4d and open condensation reaction still circulating cooling water valve 4f, and during condensation reaction, if Controlling System is according to the signal that carrys out temperature sensor in self-condensation reaction still, further judging temperature in condensation reaction still is not less than the second design temperature or judges condensation reaction still agitator 4c and stop operating over setting-up time or according to the signal that carrys out the pressure transmitter in self-condensation reaction still circulating cooling water coil 4a, judging pressure in condensation reaction still circulating cooling water coil 4a is less than the first hydraulic pressure set(ting)value and continued for first scheduled time or according to the signal of the pressure transmitter from condensation filler pipe road 102, judging pressure in condensation filler pipe road is less than the second hydraulic pressure set(ting)value and continued for second scheduled time or judge condensation reaction still temperature interlocking emergency stop push button and be pressed, start secondary temperature interlocked control, open condensation priming valve 3b, close condensation reaction still cycling hot water valve 4d and open condensation reaction still circulating cooling water valve 4f.
The production unit of the dicumyl peroxide condensation reaction providing according to above-described embodiment of the present utility model, wherein during condensation reaction, when judging whether to start one-level temperature interlocked control, if when the temperature in condensation reaction still is less than the first design temperature, continue condensation reaction.
The production unit of the dicumyl peroxide condensation reaction providing according to above-described embodiment of the present utility model, wherein during condensation reaction, when judging whether to start secondary temperature interlocked control, if Controlling System is according to the signal that carrys out temperature sensor in self-condensation reaction still, the temperature of judging in condensation reaction still is greater than the first design temperature and is less than the second design temperature, and do not meet other conditions that start secondary temperature interlocked control, start one-level temperature interlocked control, close condensation reaction still cycling hot water valve 4d and open condensation reaction still circulating cooling water valve 4f.
The production unit of the dicumyl peroxide condensation reaction providing according to above-described embodiment of the present utility model, wherein when judging whether to start secondary temperature interlocked control, if Controlling System is according to the signal that carrys out temperature sensor in self-condensation reaction still, the temperature of judging in condensation reaction still is less than the first design temperature and does not meet other conditions that start secondary temperature interlocked control, continues condensation reaction.
The production unit of the dicumyl peroxide condensation reaction providing according to above-described embodiment of the present utility model, wherein the production unit of dicumyl peroxide condensation reaction also comprises the condensation washing kettle 7 being connected with the bottom circulation of condensation reaction still 4, condensation washing kettle 7 adds alkali scale tank 9 with condensation, system vacuum pump (not shown), 10 circulations are connected condensation lye vat 11 with condensation alkali cleaning subsider, condensation alkali cleaning subsider 10 leads to and connects with condensation lye vat 11 and condensation water wash column stream 12 respectively, condensation water wash column 12 is connected with 13 circulations of condensation liquid bath, after condensation reaction finishes, by the system vacuum pump being connected with 4 circulations of condensation washing kettle, it is vacuumized, to the condensated liquid in condensation reaction still 4 is pumped in condensation washing kettle 7, thereby with the alkali lye that condensation adds in alkali scale tank 9, the condensated liquid in condensation washing kettle 7 is carried out to alkali cleaning, during alkali cleaning, open the condensation washing kettle agitator 7e in condensation washing kettle 7, after alkali cleaning finishes, at the interior quiescent settling of condensation washing kettle 7, alkali lye after layering is discharged in condensation lye vat 11 and via condensation lye vat 11 and is discharged into outside, and the condensated liquid after alkali cleaning layering is pumped in condensation alkali cleaning subsider 10 by the condensation liquid pump 14 being arranged between condensation washing kettle 7 and condensation alkali cleaning subsider 10, condensated liquid is at condensation alkali cleaning subsider 10 again after sedimentation, the alkali lye of secondary clearing is again discharged in condensation lye vat 11 and via condensation lye vat 11 and is discharged into outside, the condensated liquid of secondary clearing is again pumped in condensation water wash column by the condensation washing pump 15 being arranged between condensation alkali cleaning subsider 10 and condensation water wash column 12, utilize washing hot water in condensation water wash column 12, condensated liquid to be washed, condensated liquid after washing is discharged in condensation liquid bath 13 and stores, and hot water emission after washing is to the outside of condensation water wash column 12.
The production unit of the dicumyl peroxide condensation reaction providing according to above-described embodiment of the present utility model, wherein in alkali cleaning, during sedimentation and washing, if the temperature that Controlling System is judged in condensation reaction still is not less than the first design temperature, start one-level temperature interlocked control, close condensation reaction still cycling hot water valve and open condensation reaction still circulating cooling water valve, and if Controlling System is judged temperature in condensation reaction still and is not less than the second design temperature or judges condensation reaction still agitator and stop operating over setting-up time or judge pressure in condensation reaction still circulating cooling water coil and be less than the first hydraulic pressure set(ting)value and continued for first scheduled time or judge pressure in condensation filler pipe road and be less than the second hydraulic pressure set(ting)value and continued for second scheduled time or judge condensation reaction still temperature interlocking emergency stop push button and be pressed, start secondary temperature interlocked control, open condensation priming valve, close condensation reaction still cycling hot water valve and open condensation reaction still circulating cooling water valve.
The production unit of the dicumyl peroxide condensation reaction providing according to above-described embodiment of the present utility model, wherein during alkali cleaning, sedimentation and washing, when judging whether to start one-level temperature interlocked control, when if the temperature in condensation reaction still is less than the first design temperature, continue alkali cleaning, sedimentation or washing.
The production unit of the dicumyl peroxide condensation reaction providing according to above-described embodiment of the present utility model, wherein in alkali cleaning, during sedimentation and washing, when judging whether to start secondary temperature interlocked control, if Controlling System is according to the signal that carrys out temperature sensor in self-condensation reaction still, the temperature of judging in condensation reaction still is greater than the first design temperature and is less than the second design temperature, and do not meet other conditions that start secondary temperature interlocked control, start one-level temperature interlocked control, close condensation reaction still cycling hot water valve and open condensation reaction still circulating cooling water valve.
The production unit of the dicumyl peroxide condensation reaction providing according to above-described embodiment of the present utility model, wherein during alkali cleaning, sedimentation and washing, when judging whether to start secondary temperature interlocked control, if Controlling System is according to the signal that carrys out temperature sensor in self-condensation reaction still, the temperature of judging in condensation reaction still is less than the first design temperature and does not meet other conditions that start secondary temperature interlocked control, continues alkali cleaning, sedimentation or washing.
Fig. 1 shows according to the production unit of dicumyl peroxide condensation reaction of the present utility model.The production unit of the dicumyl peroxide condensation reaction providing according to embodiment of the present utility model is provided in more detail below in conjunction with Fig. 1.As shown in Figure 1, the production unit of dicumyl peroxide condensation reaction comprises benzylalcohol groove 1a, oxidation liquid bath 2a, benzylalcohol scale tank 1, oxidation solution scale tank 2, condensation adds tank 3, condensation reaction still 4, condensation accident groove 5, condensation condenser 6, condensation washing kettle 7, condensation vacuum buffer tank 8, condensation adds alkali scale tank 9, condensation alkali cleaning subsider 10, condensation lye vat 11, condensation water wash column 12, condensation liquid bath 13, condensation liquid pump 14, condensation washing pump 15, condensation vacuum pump 18, system vacuum pump (not shown), oxidation liquid pump 2h, static mixer 16, water-and-oil separator 17, condensation top liquid bath 20 and Controlling System (not shown).
Benzylalcohol scale tank 1 is connected with 4 circulations of condensation reaction still with the benzylalcohol feed valves 1l being arranged on benzylalcohol feeding pipeline 100 by benzylalcohol feeding pipeline 100.Oxidation solution scale tank 2 is connected with 4 circulations of condensation reaction still with the oxidation solution feed valves 2g being arranged on oxidation solution feeding pipeline 101 by oxidation solution feeding pipeline 101.Condensation adds tank 3 and is connected with 4 circulations of condensation reaction still with the condensation priming valve 3b being arranged on condensation filler pipe road 102 by condensation filler pipe road 102.Catalyzer (for example perchloric acid) is connected with 4 circulations of condensation reaction still with the catalyzer feed valves 24 being arranged on catalyzer feeding pipeline 127 by catalyzer feeding pipeline 127, and catalyzer feeding pipeline 127 is inserted in condensation reaction still 4.Condensation reaction still 4 is also connected with 6 circulations of condensation condenser by the condensation waste material pipeline 103 on its top, and condensation condenser 6 is connected with 20 circulations of condensation top liquid bath with the phlegma valve 6a being arranged on the second condenser pipe 106 by the first condenser pipe 107 with 103 tandems of condensation waste material pipeline and the second condenser pipe 106.Condensation condenser 6 is also connected with vacuum buffer tank 8 circulations with the condensation reaction still vacuum valve 4l being arranged on the first vacuum-lines 110 by the first vacuum-lines 110, and vacuum buffer tank 8 is connected with condensation vacuum pump 18 by the 3rd vacuum-lines 111.Vacuum buffer tank 8 is also connected with 7 circulations of condensation washing kettle with the condensation washing kettle condensation vacuum pump valve 7c being arranged on the second vacuum-lines 109 by the second vacuum-lines 109.
Condensation reaction still 4 is also connected with 7 circulations of condensation washing kettle with the condensation reaction still bleeder valve 4j being arranged on condensated liquid alkali cleaning pipeline 105 by condensated liquid alkali cleaning pipeline 105.Condensation reaction still 4 is also connected with bubbler 22 circulations by bubbler valve 21.In condensation reaction still 4, be also provided with condensation reaction still circulating cooling water coil 4a, circulation is connected condensation reaction still circulating cooling water coil 4a with condensation reaction still recirculated cooling water outlet valve 4g with condensation reaction still circulating cooling water inlet valve 4f, for condensation reaction still 4 being carried out to cooling condensation reaction still recirculated cooling water, by condensation reaction still circulating cooling water inlet valve 4f, is flowed into condensation reaction still circulating cooling water coil 4a and is flowed out by condensation reaction still recirculated cooling water outlet valve 4g.Condensation reaction still 4 also comprises and is arranged on its outside condensation reaction still circulating hot water chuck 4b, circulation is connected condensation reaction still circulating hot water chuck 4b with condensation reaction still circulating hot water outlet valve 4e with condensation reaction still circulating hot water inlet valve 4d, for the condensation reaction still circulating hot water that condensation reaction still 4 is heated, by condensation reaction still circulating hot water inlet valve 4d, is flowed into condensation reaction still circulating hot water chuck 4b and is flowed out by condensation reaction still circulating hot water outlet valve 4e.Condensation reaction still 4 also comprises the condensation reaction still agitator 4c being arranged on wherein.Condensation reaction still 4 carries out sampling analysis by the condensation reaction still sampling valve 4h arranging thereunder to the condensated liquid in condensation reaction still 4, to determine whether stopping condensation reaction.Condensation reaction still 4 also comprises pressure transmitter P disposed thereon, temperature sensor T and liquidometer L.On condensation reaction still circulating cooling water coil 4a, be provided with the pressure transmitter P that crosses condensation reaction still circulating cooling water pressure wherein for senses flow, and on condensation filler pipe road 102, be provided with for senses flow cross wherein for stopping the pressure transmitter P of pressure of the water of condensation reaction.In an embodiment of the present utility model, bubbler 22 is communicated with the bottom of condensation reaction still 4 by first end, and the second end of bubbler 22 is positioned at condensation reaction still 4 outsides and high and and the air communication than the height of condensation reaction still 4.In an embodiment of the present utility model, bubbler 22 is U-shaped pipe.Bubbler 22 also can adopt other mode, and this also will drop in protection domain of the present utility model.
Condensation reaction still 4 also comprises condensation reaction still temperature interlocking emergency stop push button (not shown) and condensation reaction still temperature interlocking resetting switch (not shown), condensation reaction still temperature interlocking emergency stop push button is used in the situation that the production unit of dicumyl peroxide condensation reaction occurs that emergency is pressed, thereby the water that condensation is added to the predetermined amount in tank 3 all joins in condensation reaction still 4, for stopping condensation reaction.Condensation reaction still temperature interlocking resetting switch is in the situation that the emergency of the production unit of dicumyl peroxide condensation reaction is excluded resets, thereby continues condensation reaction.
Preferably; condensation reaction still 4 is also connected with 5 circulations of condensation accident groove with the rupture disk 5a being arranged on condensation accident pipeline 104 by condensation accident pipeline 104; so that in the situation that condensation reaction still 4 is blasted; making reaction solution in condensation reaction still 4 break through rupture disk 5a is circulated in condensation accident groove 5 via condensation accident pipeline 104; condensation accident groove 5 keeps normal atmosphere, and condensation accident groove 5 for playing the effect of protection operation site in the situation that condensation reaction still 4 is blasted.
Condensation adds alkali scale tank 9 and is added alkali pipeline 108 and be arranged on condensation and add condensation alkali addition valve 9a on alkali pipeline 108 and be connected with 7 circulations of condensation washing kettle by condensation.Condensation washing kettle 7 is also connected with system vacuum pump with the condensation washing kettle vacuum pump valve 7d being arranged on the 4th vacuum-lines 128 by the 4th vacuum-lines 128.Condensation washing kettle 7 is also connected with 11 circulations of condensation lye vat through the first recycle of alkali liquor pipeline 121 by condensation washing kettle outlet valve 7a.Condensation washing kettle 7 is also collected pipeline 120 by condensation washing kettle outlet valve 7a through the first condensated liquid and is connected with 10 circulations of condensation alkali cleaning subsider with condensation alkali cleaning subsider inlet valve 10c with the condensation liquid pump 14 being arranged on the first condensated liquid collection pipeline 120.Condensation alkali cleaning subsider 10 is also connected with 11 circulations of condensation lye vat with condensation alkali cleaning subsider the first outlet valve 10a being arranged on the second recycle of alkali liquor road 112 by the second recycle of alkali liquor road 112, and wherein condensation lye vat 11 also comprises the condensation lye vat wastewater valve 11b that is arranged on the condensation lye vat blow-off valve 11a at top and is arranged on bottom.Condensation alkali cleaning subsider 10 is also washed pipeline 115 and condensation alkali cleaning subsider the second outlet valve 10b being arranged on condensated liquid washing pipeline 115 by condensated liquid, condensation washing pump 15, static mixer 16, water-and-oil separator 17 is connected with 12 circulations of condensation water wash column with condensation water wash column feed valve 12d, wherein condensation water wash column 12 is connected with 13 circulations of condensation liquid bath with the condensation water wash column surplus valve 12a being arranged on condensated liquid overflow passage 116 by condensated liquid overflow passage 116, condensation water wash column 12 also comprises side's disposed thereon condensation water wash column blow-off valve 12b and thereunder condensation water wash column wastewater valve 12c is set, condensation water wash column hot water by the first washing pipeline 118 be arranged on condensation water wash column the first hot water valve 12e on the first washing pipeline 118 and/or join in condensation water wash column 12 by the second washing pipeline 117 with 115 tandems of condensated liquid washing pipeline and condensation water wash column the second hot water valve 12f being arranged on the second washing pipeline 117, to condensated liquid is washed in condensation water wash column 12.
Be used for storing α, the benzylalcohol groove 1a of α-dimethyl benzyl alcohol by benzylalcohol metering pipeline 122, be arranged on benzylalcohol groove outlet valve 1b on benzylalcohol metering pipeline 122 and be connected with 1 circulation of benzylalcohol scale tank with benzylalcohol scale tank feed valve 1c, for the benzylalcohol of benzylalcohol groove 1a predetermined amount is joined in benzylalcohol scale tank 1.Benzylalcohol scale tank 1 is also connected with benzylalcohol groove 1a circulation with the benzylalcohol scale tank reverse flow valve 1d being arranged on benzylalcohol return line 126 by benzylalcohol return line 126, and for making benzylalcohol scale tank 1, excessive benzylalcohol is back in benzylalcohol groove 1a.Benzylalcohol groove 1a is provided with liquidometer L, for measuring the benzylalcohol amount of benzylalcohol groove 1a.Benzylalcohol scale tank 1 is provided with benzylalcohol scale tank heating water jacket (not shown), benzylalcohol scale tank circulating hot water is flowed into benzylalcohol scale tank heating water jacket and is flowed out benzylalcohol scale tank heating water jacket by benzylalcohol scale tank hot water outlet valve 1h by benzylalcohol scale tank hot water inlet valve 1g, for the benzylalcohol of benzylalcohol groove is heated.Benzylalcohol scale tank 1 is also provided with electrometer treasure W and liquidometer L, for to from flowing into benzylalcohol metering wherein.The top of benzylalcohol scale tank 1 is also provided with benzylalcohol scale tank blow-off valve 1f and benzylalcohol scale tank vacuum valve 1e, and wherein benzylalcohol scale tank vacuum valve 1e is connected with system vacuum pump, for benzylalcohol scale tank 1 is vacuumized.
For the oxidation liquid bath 2a that stores oxidation solution, by oxidation solution metering pipeline 123, oxidation liquid bath outlet valve 2b, the oxidation liquid pump 2h and the oxidation solution scale tank feed valve 2d that are arranged on oxidation solution metering pipeline 123, be connected with 2 circulations of oxidation solution scale tank, for the oxidation solution (cumene solution of hydrogen phosphide cumene) that is oxidized liquid bath 2a is pumped in oxidation solution scale tank 2 by oxidation liquid pump 2h.Oxidation solution scale tank 2 is also connected with oxidation liquid bath 2a circulation with the oxidation liquid bath reverse flow valve 2c being arranged on oxidation solution the second return line 124 with the oxidation solution scale tank surplus valve 2f and oxidation solution the second return line 124 that are arranged on oxidation solution the first return line 125 by oxidation solution the first return line 125, for the excess oxidation fluid of oxidation solution scale tank 2 is back in oxidation liquid bath 2a.Oxidation solution scale tank 2 also comprises side's disposed thereon oxidation solution scale tank blow-off valve 2e.Oxidation solution scale tank 2 is also provided with electrometer treasure W and liquidometer L, for to from flowing into oxidation solution metering wherein.
According to the production unit of dicumyl peroxide condensation reaction of the present utility model, also comprise Controlling System, Controlling System is electrically connected to each pressure transmitter P, each temperature sensor T, each electrometer treasure W, each liquidometer L, condensation reaction still circulating hot water inlet valve 4d, condensation reaction still circulating cooling water inlet valve 4f, condensation reaction still agitator 4c, condensation washing kettle agitator 7e and condensation priming valve 3b, condensation liquid pump 14, oxidation liquid pump 2h, system vacuum pump and condensation vacuum pump 18.In an embodiment of the present utility model, Controlling System is Safety instrument system SIS.
During condensation reaction, Controlling System is according to the signal that carrys out temperature sensor T in self-condensation reaction still 4, the temperature of judging in condensation reaction still is not less than the first design temperature (for example 45 ℃), start one-level temperature interlocked control,, close condensation reaction still cycling hot water valve and open condensation reaction still circulating cooling water valve, otherwise temperature in condensation reaction still does not surpass 45 ℃, continues condensation reaction.During condensation reaction, if Controlling System is according to the signal that carrys out temperature sensor T in self-condensation reaction still, judging temperature in condensation reaction still is not less than the second design temperature (for example 46 ℃) or judges condensation reaction still agitator and stop operating for example, over setting-up time (10 minutes) or according to the signal for the pressure transmitter of hydraulic pressure in sensing condensation reaction still circulating cooling water coil, judging pressure in condensation reaction still circulating cooling water coil is less than the first hydraulic pressure set(ting)value (for example 0.20MPa) and continues first scheduled time (for example 3 minutes) or according to the signal of the pressure transmitter for sensing condensation filler pipe road hydraulic pressure, judging pressure in condensation filler pipe road is less than the second hydraulic pressure set(ting)value (for example 0.20MPa) and continues second scheduled time (for example 10 minutes) or judge condensation reaction still temperature interlocking emergency stop push button and be pressed, start secondary temperature interlocked control,, open condensation priming valve, close condensation reaction still cycling hot water valve and open condensation reaction still circulating cooling water valve.Wherein, if Controlling System is according to the signal that carrys out temperature sensor T in self-condensation reaction still, the temperature of judging in condensation reaction still is greater than the first design temperature and is less than the second design temperature, and do not meet other conditions that start secondary temperature interlocked control, start one-level temperature interlocked control, close condensation reaction still cycling hot water valve and open condensation reaction still circulating cooling water valve.If the temperature that Controlling System according to the signal that carrys out temperature sensor T in self-condensation reaction still, is judged in condensation reaction still is less than the first design temperature and does not meet other conditions that start secondary temperature interlocked control, continue condensation reaction.
To introduce in detail according to the principle of work of the production unit of dicumyl peroxide condensation reaction of the present utility model below.
First, close condensation priming valve 3b and open condensation and add tank feed valve 3a, the river of predetermined amount (for example 500kg) is joined to condensation and add in tank 3.Alternatively, also can be by the joining condensation and add in tank 3 for stopping the river of the condensation reaction of condensation reaction still 4 of other predetermined amounts, and this is also in protection domain of the present utility model.
Then, benzylalcohol in benzylalcohol groove 1a meets after the requirement of condensation reaction, close benzylalcohol feed valves 1l, close benzylalcohol groove outlet valve 1b, open benzylalcohol scale tank hot water inlet valve 1g, open benzylalcohol scale tank hot water outlet valve 1h, open benzylalcohol scale tank feed valve 1c, close benzylalcohol scale tank blow-off valve 1f and open benzylalcohol scale tank vacuum pumping valve 1e, benzylalcohol scale tank 1 is vacuumized.Then, opening benzylalcohol groove outlet valve 1b utilizes pressure reduction that vacuum pump produces between benzylalcohol groove 1a and benzylalcohol scale tank 1 to benzylalcohol charging.Benzylalcohol liquid level in benzylalcohol scale tank 1 reaches after predetermined benzylalcohol liquid level, closes benzylalcohol scale tank feed valve 1c, closes benzylalcohol scale tank vacuum pumping valve 1e and opens benzylalcohol scale tank blow-off valve 1f.If the benzylalcohol liquid level in benzylalcohol scale tank 1 surpasses predetermined benzylalcohol liquid level, open benzylalcohol scale tank blow-off valve 1f, and open benzylalcohol scale tank reverse flow valve 1d, in benzylalcohol scale tank 1, the liquid level of remaining benzylalcohol reaches after predetermined benzylalcohol liquid level, closes benzylalcohol scale tank reverse flow valve 1d and benzylalcohol groove outlet valve 1b.By the electrometer treasure W on benzylalcohol scale tank 1 and liquidometer L, the benzylalcohol in benzylalcohol scale tank 1 is measured.Then, open benzylalcohol scale tank sampling valve 1j and analyze its weight percent content (for example the weight percent content of CA is not less than 90%) from a certain amount of benzylalcohol of benzylalcohol scale tank 1 taking-up.By regulating benzylalcohol scale tank hot water inlet valve 1g and benzylalcohol scale tank hot water outlet valve 1h to regulate the flow of benzylalcohol scale tank circulating hot water, to the temperature of benzylalcohol scale tank 1 interior benzylalcohol is controlled between 50 ℃ ~ 60 ℃ during charging and analysis benzylalcohol scale tank 1 is carried out.
Then, close communicating valve between oxidation liquid pump 2h and reduction kettle (for carrying out therein the reduction reaction of dicumyl peroxide), close oxidation solution feed valves 2g, open oxidation solution scale tank blow-off valve 2e, open oxidation liquid bath outlet valve 2b, open oxidation liquid bath reverse flow valve 2c, open oxidation solution scale tank feed valve 2d, open oxidation solution scale tank surplus valve 2f and start oxidation liquid pump 2h, the oxidation solution of predetermined amount is pumped in oxidation solution scale tank 2 under the effect that is oxidized liquid pump 2h from oxidation liquid bath 2a.At the electrometer treasure W by oxidation solution scale tank 2 and liquidometer L, determine that the oxidation solution liquid level in oxidation solution scale tank 2 reaches after predetermined oxidation solution liquid level, close oxidation solution scale tank feed valve 2d, close oxidation solution scale tank surplus valve 2f, stop being oxidized liquid pump 2h and close oxidation liquid bath outlet valve 2b, close oxidation liquid bath reverse flow valve 2c.When oxidation solution in oxidation solution scale tank 2 is excessive, stop being oxidized liquid pump 2h and oxidation solution scale tank feed valve 2d, excessive oxidation solution is back in oxidation liquid bath 2a by oxidation solution scale tank surplus valve 2f and oxidation liquid bath reverse flow valve 2c.During 2 chargings of oxidation solution scale tank, be held open oxidation solution scale tank blow-off valve 2e always.After completing 2 chargings of oxidation solution scale tank, in 21 pairs of oxidation solution scale tanks 2 of unlatching oxidation solution scale tank sampling valve, oxidation solution samples and analyzes the weight percent content of oxidation solution in oxidation solution scale tank 2.
Then, on the basis that benzylalcohol and hydrogen phosphide cumene are measured and analyzed, according to carry out dicumyl peroxide condensation reaction time hydrogen phosphide cumene and benzylalcohol mol ratio be 1:(0.95 ~ 1), reaffirm whether the charging capacity of benzylalcohol and the charging capacity of hydrogen phosphide cumene meet to set requirement.If meet to set, require, according to following steps, feed intake.Otherwise repeat above-mentioned steps and adjust the charging capacity of benzylalcohol and the charging capacity of hydrogen phosphide cumene.According to carry out dicumyl peroxide condensation reaction time hydrogen phosphide cumene oxidation solution charging capacity and while carrying out condensation reaction perchloric acid catalysis agent and the weight ratio (being for example 0.076:100) of hydrogen phosphide cumene determine the charging capacity of catalyzer.
Then, open condensation condenser refrigerating fulid inlet valve 6a, open condensation condenser refrigerating fulid outlet valve 6b, open condensation reaction still agitator 4c, open condensation vacuum pump 18 and open condensation reaction still vacuum valve 4l.The condensation condenser 6 communicating with each other via 8 pairs of condensation vacuum buffer tanks by condensation vacuum pump 18, condensation top liquid bath 20 and condensation reaction still 4 vacuumize.Then, when making condensation reaction still 4 inside be pumped down to the vacuum limit (as 30MPa) by condensation vacuum pump 18, open benzylalcohol feed valves 1l, the benzylalcohol after analyzing and measuring is joined in condensation reaction still 4 through Bian alcohol feeding pipeline 100 by benzylalcohol scale tank 1.Then, the charging capacity of the benzylalcohol in condensation reaction still 4 reaches after the mouth of pipe of catalyzer feeding pipeline 127, opening catalyzer feed valves 24 joins the catalyzer (for example perchloric acid) after analyzing and measuring in condensation reaction still 4, after catalyzer has fed intake, close catalyzer feed valves 24 and after benzylalcohol has fed intake, close benzylalcohol feed valves 1l.Then, open oxidation solution scale tank blow-off valve 2e, open oxidation solution feed valves 2g, the oxidation solution after analyzing and measuring is joined in condensation reaction still 4, after oxidation solution has fed intake, close oxidation solution feed valves 2g.Whole, feed intake in process, if had extremely, ascertain the reason and make respective handling.
Then, after having fed intake, open bubbler valve 21, by condensation vacuum pump 18 and bubbler valve 21, the pressure in condensation reaction still 4 is adjusted in the scope of-0.06 ~-0.02MPa.Then, open condensation reaction still circulating hot water inlet valve 4d, condensation reaction still circulating hot water outlet valve 4e, condensation reaction still circulating cooling water inlet valve 4f and condensation reaction still recirculated cooling water outlet valve 4g, for example, so that within first scheduled time of closing oxidation solution feed valves 2g (15 minutes), the temperature in condensation reaction still 4 is controlled in the scope of 42 ℃ ~ 45 ℃ and for example, within second scheduled time of certainly opening bubbler valve 21 (1 hour) temperature in condensation reaction still 4 is controlled in the scope of 42 ℃ ~ 45 ℃.Then, from benzylalcohol, for example feed intake, after the 3rd scheduled time (1 hour) starting, at set intervals to the condensated liquid sampling analysis in condensation reaction still 4, when in condensated liquid, the weight percent content of dicumyl peroxide is between 0.2% ~ 1.5%, can stop condensation reaction, now, opening condensation priming valve 3b adds water in tank 3 by condensation and all joins in condensation reaction still 4 and stop condensation reaction, and close condensation reaction still circulating hot water inlet valve 4d, condensation reaction still circulating hot water outlet valve 4e, condensation reaction still circulating cooling water inlet valve 4f, condensation reaction still recirculated cooling water outlet valve 4g and bubbler valve 21 and stop condensation vacuum pump 18.During condensation reaction, a part of gaseous phase materials that vacuum bubbling is taken out of (comprising water and isopropyl benzene) condenses to condensation condenser 6 by condensation pipeline 103, and another part gaseous state isopropyl benzene and water are collected in condensation top liquid bath 20 by condensation pipeline 103 with the first condenser pipe 107 of its tandem after condensation, the condensed a part of gaseous state isopropyl benzene and the water that are collected in condensation condenser 6 are collected in condensation top liquid bath 20 with the condensation condenser bleeder valve 6c being arranged on the second condenser pipe 106 by the second condenser pipe 106.After condensation reaction finishes, be collected in condensed gaseous state isopropyl benzene in condensation top liquid bath 20 and water and by top fluid dewatering groove feed valve 20b, collect concentrate top fluid dewatering groove (not shown) and carry out concentrate.Wherein condensation top liquid bath outlet valve 20a is as Redundancy Design, to play redundancy protecting effect when top fluid dewatering groove feed valve 20b damages.
Then, close condensation washing kettle outlet valve 7a, close condensation washing kettle condensation vacuum pump valve 7c, close condensation washing kettle blow-off valve 7b, open condensation washing kettle system vacuum pump valve 7d and open condensation washing kettle agitator 7e, by system vacuum pump (not shown), condensation washing kettle 7 is vacuumized, to produce pressure reduction between condensation reaction still 4 and condensation washing kettle 7, thereby the condensated liquid in the condensation reaction still 4 after condensation reaction is finished is pumped in condensation washing kettle 7 by condensated liquid alkali cleaning pipeline 105 and condensation reaction still bleeder valve 4j disposed thereon.Then, open and to be arranged on condensation and to add condensation alkali addition valve 9a on alkali pipeline 108 and condensation is added to alkali lye (for example sodium hydroxide solution) in alkali scale tank 9 join in condensation washing kettle 7 condensated liquid is wherein washed.Pass condensation alkali addition valve 9a after condensation adds liquid caustic soda in alkali scale tank 9 all to add condensation washing kettle 7.Condensated liquid in condensation reaction still is all pumped into after condensation washing kettle 7, close condensation reaction still bleeder valve 4j, halt system vacuum pump, open the blow-off valve 7b on condensation washing kettle 7, after stirring fully, stop condensation washing kettle agitator 7e, the quiescent settling scheduled time, make condensated liquid and alkali lye layering, alkali lye after layering is recovered to condensation lye vat 11 by condensation washing kettle outlet valve 7a and the first recycle of alkali liquor road 121, in condensation washing kettle, add alkali repetition alkali cleaning 2 ~ 4 times again, the condensation lye vat blow-off valve 11a of condensation lye vat 11 tops and condensation lye vat wastewater valve 11b open during this period, alkali lye in condensation lye vat 11 can discharge by condensation lye vat wastewater valve 11b.Condensated liquid after layering is collected pipeline 120 and condensation liquid pump 14 disposed thereon and condensation alkali cleaning subsider inlet valve 10c by condensation washing kettle outlet valve 7a and the first condensated liquid and is pumped in condensation alkali cleaning subsider 10 and carries out secondary settlement, keep during this period condensation alkali cleaning subsider the first outlet valve 10a and condensation alkali cleaning subsider the second outlet valve 10b to close, and keep alkali cleaning subsider blow-off valve to open.After all condensated liquids are all pumped in condensation alkali cleaning subsider 10 in condensation washing kettle 7, close condensation washing kettle outlet valve 7a, close condensation alkali cleaning subsider inlet valve 10c and stop condensation liquid pump 14.After condensation alkali cleaning subsider 10 secondary settlements, make condensated liquid and remaining alkali lye layering, the residue alkali lye after layering is discharged in condensation lye vat 11 and by condensation lye vat wastewater valve 11b and is discharged by condensation alkali cleaning subsider the first outlet valve 10a.Condensated liquid after layering is washed pipeline 115 by condensated liquid and is connected on condensation water wash column 12 by the condensation washing pump 15, static mixer 16, water-and-oil separator 17 and the condensation water wash column feed valve 12d circulation that are arranged on condensated liquid washing pipeline 115.Static mixer 16 is for hot wash-water is mixed with condensated liquid, and water-and-oil separator 17 is for filtering the solid impurity of condensated liquid, for example iron rust.Condensated liquid in condensation alkali cleaning subsider 10 is all being pumped into after condensation water wash column 12, opening condensation water wash column the first hot water valve 12e and/or condensation water wash column the second hot water valve 12f utilizes hot water to wash the condensated liquid in condensation water wash column 12, during washing, keep condensation water wash column wastewater valve 12c to close and keep condensation water wash column blow-off valve 12b to open, after condensated liquid is washed, open condensation water wash column surplus valve 12a, condensated liquid after washing is overflowed in condensation liquid bath 13 with the condensation water wash column surplus valve 12a being arranged on condensated liquid overflow passage 116 by condensated liquid overflow passage 116, and washing after waste water by condensation water wash column wastewater valve 12c, discharge.
Fig. 2 shows according to the production method of dicumyl peroxide condensation reaction of the present utility model.To describe the production method of dicumyl peroxide condensation reaction in detail below:
Step 100: start according to the production method of dicumyl peroxide condensation reaction of the present utility model.
Step 102: the river of predetermined amount is joined to condensation and add in tank.Specifically, close condensation priming valve 3b and open condensation and add tank feed valve 3a, by the river of predetermined amount for example 500kg join condensation and add in tank 3.
Step 104: the benzylalcohol of predetermined amount is joined in benzylalcohol scale tank and to its metering and analysis.Specifically, close benzylalcohol feed valves 1l, close benzylalcohol groove outlet valve 1b, open benzylalcohol scale tank hot water inlet valve 1g, open benzylalcohol scale tank hot water outlet valve 1h, open benzylalcohol scale tank feed valve 1c, close benzylalcohol scale tank blow-off valve 1f and open benzylalcohol scale tank vacuum pumping valve 1e, benzylalcohol scale tank 1 is vacuumized.Then, opening benzylalcohol groove outlet valve 1b utilizes pressure reduction that vacuum pump produces between benzylalcohol groove 1a and benzylalcohol scale tank 1 to benzylalcohol charging.Benzylalcohol liquid level in benzylalcohol scale tank 1 reaches after predetermined benzylalcohol liquid level, closes benzylalcohol scale tank feed valve 1c, closes benzylalcohol scale tank vacuum pumping valve 1e and opens benzylalcohol scale tank blow-off valve 1f.If the benzylalcohol liquid level in benzylalcohol scale tank 1 surpasses predetermined benzylalcohol liquid level, open benzylalcohol scale tank reverse flow valve 1d, in benzylalcohol scale tank 1, the liquid level of remaining benzylalcohol reaches after predetermined benzylalcohol liquid level, closes benzylalcohol scale tank reverse flow valve 1d and benzylalcohol groove outlet valve 1b.By the electrometer treasure W on benzylalcohol scale tank 1 and liquidometer L, the benzylalcohol in benzylalcohol scale tank 1 is measured.Then, open benzylalcohol scale tank sampling valve 1j and analyze its weight percent content (for example the weight percent content of CA is not less than 90%) from a certain amount of benzylalcohol of benzylalcohol scale tank 1 taking-up.By regulating benzylalcohol scale tank hot water inlet valve 1g and benzylalcohol scale tank hot water outlet valve 1h to regulate the flow of benzylalcohol scale tank circulating hot water, to the temperature of benzylalcohol scale tank 1 interior benzylalcohol is controlled between 50 ℃ ~ 60 ℃ during charging and analysis benzylalcohol scale tank 1 is carried out.
Step 106: the oxidation solution of predetermined amount is joined in oxidation solution scale tank and to its metering and analysis.Specifically, for the oxidation liquid bath 2a that stores oxidation solution, by oxidation solution metering pipeline 123, oxidation liquid bath outlet valve 2b, the oxidation liquid pump 2h and the oxidation solution scale tank feed valve 2d that are arranged on oxidation solution metering pipeline 123, be connected with 2 circulations of oxidation solution scale tank, for the oxidation solution (cumene solution of hydrogen phosphide cumene) that is oxidized liquid bath 2a is pumped in oxidation solution scale tank 2 by oxidation liquid pump 2h.Oxidation solution scale tank 2 is also connected with oxidation liquid bath 2a circulation with the oxidation liquid bath reverse flow valve 2c being arranged on oxidation solution the second return line 124 with the oxidation solution scale tank surplus valve 2f and oxidation solution the second return line 124 that are arranged on oxidation solution the first return line 125 by oxidation solution the first return line 125, for the excess oxidation fluid of oxidation solution scale tank 2 is back in oxidation liquid bath 2a.Oxidation solution scale tank 2 also comprises side's disposed thereon oxidation solution scale tank blow-off valve 2e.Oxidation solution scale tank 2 is also provided with electrometer treasure W and liquidometer L, for to from flowing into oxidation solution metering wherein.
Step 108: before feeding intake, according to the mol ratio of carrying out hydrogen phosphide cumene and the benzylalcohol of condensation reaction, whether the charging capacity of again checking oxidation solution and benzylalcohol meets condensation reaction requirement.Specifically, according to carry out dicumyl peroxide condensation reaction time hydrogen phosphide cumene and benzylalcohol mol ratio be 1:(0.95 ~ 1), reaffirm whether the charging capacity of benzylalcohol and the charging capacity of hydrogen phosphide cumene meet to set requirement.If meet to set and require execution step 110.Otherwise execution step 109: the charging capacity of oxidation solution in the charging capacity of benzylalcohol and oxidation solution scale tank 2 in adjustment benzylalcohol scale tank 1.
Step 110: during according to condensation reaction, the weight ratio of the charging capacity of oxidation solution and catalyzer and hydrogen phosphide cumene oxidation solution is determined the charging capacity of catalyzer.In the utility model, in oxidation solution, the weight percent content of hydrogen phosphide cumene is 40 ~ 70%, be weight percentage 50% ~ 70% perchloric acid of catalyzer, and the weight ratio of catalyzer and hydrogen phosphide cumene is: 0.076:100.It should be noted that, also can adopt the weight ratio of other acid catalyst and catalyzer and hydrogen phosphide cumene, and this is also in scope of the present utility model.
Step 112: make the refrigerating fulid condensation shrinkage of flowing through close condenser, and condensation reaction still is vacuumized, metering and benzylalcohol, catalyzer and the oxidation solution analyzed are joined in condensation reaction still successively.Specifically, open condensation condenser refrigerating fulid inlet valve 6a, open condensation condenser refrigerating fulid outlet valve 6b, open condensation reaction still agitator 4c, open condensation vacuum pump 18 and open condensation reaction still vacuum valve 4l.The condensation condenser 6 communicating with each other via 8 pairs of condensation vacuum buffer tanks by condensation vacuum pump 18, condensation top liquid bath 20 and condensation reaction still 4 vacuumize.Then, when making condensation reaction still 4 inside be pumped down to the vacuum limit (as 30MPa) by condensation vacuum pump 18, open benzylalcohol feed valves 1l, the benzylalcohol after analyzing and measuring is joined in condensation reaction still 4 through Bian alcohol feeding pipeline 100 by benzylalcohol scale tank 1.Then, the charging capacity of the benzylalcohol in condensation reaction still 4 reaches after the mouth of pipe of catalyzer feeding pipeline 127, opening catalyzer feed valves 24 joins the catalyzer (for example perchloric acid) after analyzing and measuring in condensation reaction still 4, after catalyzer has fed intake, close catalyzer feed valves 24 and after benzylalcohol has fed intake, close benzylalcohol feed valves 1l.Then, open oxidation solution scale tank blow-off valve 2e, open oxidation solution feed valves 2g, the oxidation solution after analyzing and measuring is joined in condensation reaction still 4, after oxidation solution has fed intake, close oxidation solution feed valves 2g.Whole, feed intake in process, if had extremely, ascertain the reason and make respective handling.
Step 114: carry out condensation reaction and stop condensation reaction in condensation reaction still, a part of gaseous state isopropyl benzene and the direct condensation of water during condensation reaction are collected in the liquid bath of condensation top, and another part gaseous state isopropyl benzene during condensation reaction and water are also collected in the liquid bath of condensation top after via condensation condenser condenses.After having fed intake, open bubbler valve 21, by condensation vacuum pump 18 and bubbler valve 21, the pressure in condensation reaction still 4 is adjusted in the scope of-0.06 ~-0.02MPa.Then, open condensation reaction still circulating hot water inlet valve 4d, condensation reaction still circulating hot water outlet valve 4e, condensation reaction still circulating cooling water inlet valve 4f and condensation reaction still recirculated cooling water outlet valve 4g, for example, so that within first scheduled time of closing oxidation solution feed valves 2g (15 minutes), the temperature in condensation reaction still 4 is controlled in the scope of 42 ℃ ~ 45 ℃ and for example, within second scheduled time of certainly opening bubbler valve 21 (1 hour) temperature in condensation reaction still 4 is controlled in the scope of 42 ℃ ~ 45 ℃.Then, from benzylalcohol, for example feed intake, after the 3rd scheduled time (1 hour) starting, at set intervals to the condensated liquid sampling analysis in condensation reaction still 4, when in condensated liquid, the weight percent content of dicumyl peroxide is between 0.2% ~ 1.5%, can stop condensation reaction, now, opening condensation priming valve 3b adds water in tank 3 by condensation and all joins in condensation reaction still 4 and stop condensation reaction, and close condensation reaction still circulating hot water inlet valve 4d, condensation reaction still circulating hot water outlet valve 4e, condensation reaction still circulating cooling water inlet valve 4f, condensation reaction still recirculated cooling water outlet valve 4g and bubbler valve 21 and stop condensation vacuum pump 18.During condensation reaction, a part of gaseous state material (comprising water and isopropyl benzene) that vacuum bubbling is taken out of condenses to condensation condenser 6 by condensation pipeline 103, and another part gaseous state material is collected in condensation top liquid bath 20 by condensation pipeline 103 with the first condenser pipe 107 of its tandem after condensation, the condensed a part of gaseous state isopropyl benzene and the water that are collected in condensation condenser 6 are collected in condensation top liquid bath 20 with the condensation condenser bleeder valve 6c being arranged on the second condenser pipe 106 by the second condenser pipe 106.After condensation reaction finishes, be collected in condensed gaseous state isopropyl benzene in condensation top liquid bath 20 and water and by top fluid dewatering groove feed valve 20b, collect concentrate top fluid dewatering groove (not shown) and carry out concentrate.
Step 116: condensated liquid is pumped in condensation washing kettle and is washed, to condensation lye vat and by its discharge, condensated liquid is pumped into condensation water wash column via condensation alkali cleaning subsider and washes recycle of alkali liquor, condensated liquid after washing is collected condensation liquid bath via condensation washing top of tower, and waste water after washing is via the discharge of condensation washing tower bottom.Specifically, after condensation reaction finishes, close condensation washing kettle outlet valve 7a, close condensation washing kettle condensation vacuum pump valve 7c, close condensation washing kettle blow-off valve 7b, open condensation washing kettle system vacuum pump valve 7d and open condensation washing kettle agitator 7e, by system vacuum pump (not shown), condensation washing kettle 7 is vacuumized, to produce pressure reduction between condensation reaction still 4 and condensation washing kettle 7, thereby the condensated liquid in the condensation reaction still 4 after condensation reaction is finished is pumped in condensation washing kettle 7 by condensated liquid alkali cleaning pipeline 105 and condensation reaction still bleeder valve 4j disposed thereon.Then, open and to be arranged on condensation and to add condensation alkali addition valve 9a on alkali pipeline 108 and condensation is added to alkali lye (for example sodium hydroxide solution) in alkali scale tank 9 join in condensation washing kettle 7 condensated liquid is wherein washed.Pass condensation alkali addition valve 9a after condensation adds liquid caustic soda in alkali scale tank 9 all to add condensation washing kettle 7.Condensated liquid in condensation reaction still is all pumped into after condensation washing kettle 7, close condensation reaction still bleeder valve 4j, halt system vacuum pump, open the blow-off valve 7b on condensation washing kettle 7, after stirring fully, stop condensation washing kettle agitator 7e, the quiescent settling scheduled time, make condensated liquid and alkali lye layering, alkali lye after layering is recovered to condensation lye vat 11 by condensation washing kettle outlet valve 7a and the first recycle of alkali liquor road 121, in condensation washing kettle, add alkali repetition alkali cleaning 2 ~ 4 times again, the condensation lye vat blow-off valve 11a of condensation lye vat 11 tops and condensation lye vat wastewater valve 11b open during this period, alkali lye in condensation lye vat 11 can discharge by condensation lye vat wastewater valve 11b.Condensated liquid after layering is collected pipeline 120 and condensation liquid pump 14 disposed thereon and condensation alkali cleaning subsider inlet valve 10c by condensation washing kettle outlet valve 7a and the first condensated liquid and is pumped in condensation alkali cleaning subsider 10 and carries out secondary settlement, keep during this period condensation alkali cleaning subsider the first outlet valve 10a and condensation alkali cleaning subsider the second outlet valve 10b to close, and keep alkali cleaning subsider blow-off valve to open.After all condensated liquids are all pumped in condensation alkali cleaning subsider 10 in condensation washing kettle 7, close condensation washing kettle outlet valve 7a, close condensation alkali cleaning subsider inlet valve 10c and stop condensation liquid pump 14.After condensation alkali cleaning subsider 10 secondary settlements, make condensated liquid and remaining alkali lye layering, the residue alkali lye after layering is discharged in condensation lye vat 11 and by condensation lye vat wastewater valve 11b and is discharged by condensation alkali cleaning subsider the first outlet valve 10a.Condensated liquid after layering is washed pipeline 115 by condensated liquid and is connected on condensation water wash column 12 by the condensation washing pump 15, static mixer 16, water-and-oil separator 17 and the condensation water wash column feed valve 12d circulation that are arranged on condensated liquid washing pipeline 115.Static mixer 16 is for hot wash-water is mixed with condensated liquid, and water-and-oil separator 17 is for filtering the solid impurity of condensated liquid, for example iron rust.
Step 118: finish according to the production method of dicumyl peroxide condensation reaction of the present utility model.
During according to step 114 of the present utility model, during condensation reaction, for example, if the temperature that Controlling System is judged in condensation reaction still is not less than the first design temperature (45 ℃), start one-level temperature interlocked control, that is, close condensation reaction still cycling hot water valve and open condensation reaction still circulating cooling water valve.Otherwise the temperature that Controlling System is judged in condensation reaction still does not surpass 45 ℃, continues condensation reaction.During condensation reaction, for example, for example, for example, for example, for example, if Controlling System is judged temperature in condensation reaction still and is not less than the second design temperature (46 ℃) or judges condensation reaction still agitator and for example stop operating, over setting-up time (10 minutes) or judge pressure in condensation reaction still circulating cooling water coil and be less than the first hydraulic pressure set(ting)value (0.20MPa) and continue first scheduled time (3 minutes) or judge pressure in condensation filler pipe road and be less than the second hydraulic pressure set(ting)value (0.20MPa) and continue second scheduled time (10 minutes) or judge condensation reaction still temperature interlocking emergency stop push button and be pressed, start secondary temperature interlocked control, , open condensation priming valve, close condensation reaction still cycling hot water valve and open condensation reaction still circulating cooling water valve.Wherein, if the temperature that Controlling System is judged in condensation reaction still is greater than the first design temperature and is less than the second design temperature, and do not meet other conditions that start secondary temperature interlocked control, start one-level temperature interlocked control, close condensation reaction still cycling hot water valve and open condensation reaction still circulating cooling water valve.If the temperature that Controlling System is judged in condensation reaction still is less than the first design temperature and does not meet other conditions that start secondary temperature interlocked control, continue condensation reaction.
During according to step 116 of the present utility model, during alkali cleaning, sedimentation and washing, for example, if the temperature that Controlling System is judged in condensation reaction still is not less than the first design temperature (45 ℃), start one-level temperature interlocked control, that is, close condensation reaction still cycling hot water valve and open condensation reaction still circulating cooling water valve.Otherwise the temperature that Controlling System is judged in condensation reaction still does not surpass 45 ℃, continues alkali cleaning, sedimentation or washing.In alkali cleaning, during sedimentation and washing, for example, for example, for example, for example, for example, if Controlling System is judged temperature in condensation reaction still and is not less than the second design temperature (46 ℃) or judges condensation reaction still agitator and for example stop operating, over setting-up time (10 minutes) or judge pressure in condensation reaction still circulating cooling water coil and be less than the first hydraulic pressure set(ting)value (0.20MPa) and continue first scheduled time (3 minutes) or judge pressure in condensation filler pipe road and be less than the second hydraulic pressure set(ting)value (0.20MPa) and continue second scheduled time (10 minutes) or judge condensation reaction still temperature interlocking emergency stop push button and be pressed, start secondary temperature interlocked control, , open condensation priming valve, close condensation reaction still cycling hot water valve and open condensation reaction still circulating cooling water valve.Wherein, if the temperature that Controlling System is judged in condensation reaction still is greater than the first design temperature and is less than the second design temperature, and do not meet other conditions that start secondary temperature interlocked control, start one-level temperature interlocked control, close condensation reaction still cycling hot water valve and open condensation reaction still circulating cooling water valve.If the temperature that Controlling System is judged in condensation reaction still is less than the first design temperature and does not meet other conditions that start secondary temperature interlocked control, continue alkali cleaning, sedimentation and washing.
According to the advantage of the production unit of dicumyl peroxide condensation reaction of the present utility model and method, be, owing to adopting firsts and seconds temperature interlocked control during condensation reaction, thereby guaranteed that condensation reaction produces safely and reliably by operation.
According to being also advantageous in that of the production unit of dicumyl peroxide condensation reaction of the present utility model and method, the waste material that to reduce people be mishandle, reclaimed condensation reaction (for example, waste material is gaseous state isopropyl benzene and water) reduced material consumption, improved the utilization ratio of hydrogen phosphide cumene, improve quality product, improved product income.
Claims (7)
1. a production unit for dicumyl peroxide condensation reaction, it comprises:
Condensation adds tank, accommodates for stopping the water of the predetermined amount of condensation reaction;
Benzylalcohol scale tank, accommodates the benzylalcohol for the predetermined amount of condensation reaction;
Oxidation solution scale tank, accommodates the oxidation solution for the predetermined amount of condensation reaction;
Condensation condenser, carries out condensation for the gaseous state isopropyl benzene to condensation reaction and water;
Catalyst feed pipeline, for joining condensation reaction still by the catalyzer of predetermined amount; And
Condensation reaction still, it adds tank with condensation respectively, benzylalcohol scale tank, oxidation solution scale tank and catalyst feed pipeline circulation connect, condensation adds tank and is connected with the circulation of condensation reaction still with the condensation priming valve being arranged on condensation filler pipe road by condensation filler pipe road, condensation reaction still is also connected with the circulation of condensation vacuum buffer tank by condensation condenser, condensation vacuum buffer tank is also connected with condensation vacuum pump, condensation vacuum pump is used for condensation condenser, condensation vacuum buffer tank and condensation reaction still vacuumize, in condensation reaction still, be also provided with condensation reaction still circulating cooling water coil and condensation reaction still agitator, condensation reaction still is also provided with condensation reaction still circulating hot water chuck outward, circulation is connected condensation reaction still circulating cooling water coil with condensation reaction still recirculated cooling water outlet valve with condensation reaction still circulating cooling water inlet valve, circulation is connected condensation reaction still circulating hot water chuck with condensation reaction still circulating hot water outlet valve with condensation reaction still circulating hot water inlet valve, the benzylalcohol of predetermined amount in benzylalcohol scale tank, the catalyzer of predetermined amount, in oxidation solution scale tank, the oxidation solution of predetermined amount is dosed into successively and in condensation reaction still, carries out condensation reaction, condensation reaction still circulating cooling water coil is used for making condensation reaction still recirculated cooling water to pass through wherein, condensation reaction still circulating hot water chuck is used for making condensation reaction still circulating hot water to pass through wherein,
Condensation top liquid bath, circulation is connected condensation top liquid bath with condensation condenser with condensation reaction still, after a part of gaseous state isopropyl benzene that condensation reaction produces and water condensation, directly collect in the liquid bath of condensation top, and another part gaseous state isopropyl benzene that condensation reaction produces and water are collected in the liquid bath of condensation top after by condensation condenser condenses; It is characterized in that, Controlling System, it is with temperature sensor in condensation reaction still, condensation reaction still agitator, be electrically connected to for the pressure transmitter of hydraulic pressure in sensing condensation filler pipe road, pressure transmitter, condensation priming valve, condensation reaction still circulating hot water inlet valve, condensation reaction still circulating cooling water inlet valve and condensation reaction still temperature interlocking emergency stop push button for hydraulic pressure in condensation reaction still circulating cooling water coil.
2. the production unit of dicumyl peroxide condensation reaction according to claim 1, it is characterized in that, the production unit of dicumyl peroxide condensation reaction also comprises top fluid dewatering groove, and the condensed waste material of collecting in the liquid bath of condensation top is discharged in the fluid dewatering groove of top and carries out concentrate.
3. the production unit of dicumyl peroxide condensation reaction according to claim 1, it is characterized in that, the production unit of dicumyl peroxide condensation reaction also comprises the condensation washing kettle being connected with the bottom circulation of condensation reaction still, condensation washing kettle adds alkali scale tank, system vacuum pump, condensation lye vat with condensation, and circulation is connected with condensation alkali cleaning subsider, condensation alkali cleaning subsider is connected with the circulation of condensation lye vat and condensation water wash column respectively, and condensation water wash column and condensated liquid concentrated flow lead to and connect.
4. the production unit of dicumyl peroxide condensation reaction according to claim 1; it is characterized in that; the production unit of dicumyl peroxide condensation reaction also comprises condensation accident groove; in the situation that condensation reaction still is blasted; reaction solution in condensation reaction still can be filled in condensation accident groove, to protect condensation reaction on-the-spot.
5. the production unit of dicumyl peroxide condensation reaction according to claim 3, it is characterized in that, the production unit of dicumyl peroxide condensation reaction also comprises static mixer and the water-and-oil separator being successively set between condensation washing pump and condensation water wash column, wherein static mixer is used for making to wash hot water and mixes with condensated liquid, and water-and-oil separator is for to filtering the solid impurity of condensated liquid.
6. the production unit of dicumyl peroxide condensation reaction according to claim 1, it is characterized in that, benzylalcohol scale tank and benzylalcohol concentrated flow lead to and connect, for the benzylalcohol of the predetermined amount for condensation reaction of benzylalcohol groove is joined to benzylalcohol scale tank, oxidation solution scale tank and oxidation solution concentrated flow lead to and connect, for the oxidation solution of the predetermined amount for condensation reaction of oxidation liquid bath is joined to oxidation solution scale tank.
7. the production unit of dicumyl peroxide condensation reaction according to claim 1, it is characterized in that, benzylalcohol scale tank and oxidation solution scale tank include electrometer treasure separately, liquidometer and sampling valve, the electrometer treasure of benzylalcohol scale tank and liquidometer are for measuring the benzylalcohol of benzylalcohol scale tank, and the electrometer treasure of oxidation solution scale tank and liquidometer are for the oxidation solution metering to oxidation solution scale tank, the sampling valve of benzylalcohol scale tank samples and analyzes the weight percent content of benzylalcohol for the benzylalcohol to after metering, the sampling valve of oxidation solution scale tank samples and analyzes the weight percent content of oxidation solution for the oxidation solution to after metering.
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| CN201320305036.1U CN203715541U (en) | 2013-05-30 | 2013-05-30 | Production equipment for dicumyl peroxide condensation reaction |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104860861A (en) * | 2015-04-01 | 2015-08-26 | 中石化上海工程有限公司 | Production method for dicumyl peroxide (DCP) |
| CN105294529A (en) * | 2015-10-12 | 2016-02-03 | 中石化上海工程有限公司 | Energy-saving type dicumyl peroxide (DCP) device condensation reaction method |
| CN109942471A (en) * | 2019-04-01 | 2019-06-28 | 江苏道明化学有限公司 | A kind of DCP condensation process flow |
-
2013
- 2013-05-30 CN CN201320305036.1U patent/CN203715541U/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104860861A (en) * | 2015-04-01 | 2015-08-26 | 中石化上海工程有限公司 | Production method for dicumyl peroxide (DCP) |
| CN105294529A (en) * | 2015-10-12 | 2016-02-03 | 中石化上海工程有限公司 | Energy-saving type dicumyl peroxide (DCP) device condensation reaction method |
| CN105294529B (en) * | 2015-10-12 | 2017-05-24 | 中石化上海工程有限公司 | Energy-saving type dicumyl peroxide (DCP) device condensation reaction method |
| CN109942471A (en) * | 2019-04-01 | 2019-06-28 | 江苏道明化学有限公司 | A kind of DCP condensation process flow |
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