CN203764265U - Reduction-condensation combined reaction device - Google Patents
Reduction-condensation combined reaction device Download PDFInfo
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- CN203764265U CN203764265U CN201420193355.2U CN201420193355U CN203764265U CN 203764265 U CN203764265 U CN 203764265U CN 201420193355 U CN201420193355 U CN 201420193355U CN 203764265 U CN203764265 U CN 203764265U
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Abstract
The utility model discloses a reduction-condensation combined reaction device. The reduction-condensation combined reaction device comprises a sodium sulfide dissolving kettle, a reaction kettle, a solution pump, a washing material discharging pump, a condenser, a condensate tank, a water suction tank and a sodium sulfide solution pipeline, wherein the sodium sulfide dissolving kettle is connected with the sodium sulfide solution pipeline; the sodium sulfide solution pipeline is connected with the solution pump; the solution pump is respectively connected with the sodium sulfide dissolving kettle and the reaction kettle through pipelines; a water inlet of the reaction kettle is connected with the water suction tank through a pipeline; a discharging opening in the bottom of the reaction kettle is connected with the washing discharging pump; an air inlet is connected with a sampling valve group; the top of the reaction kettle is connected with a vacuum pipeline; the vacuum pipeline is connected with the sampling valve group and the condenser; the condenser is respectively connected with a vacuum system and the condensate tank through pipelines; a perchloric acid charging opening is formed in the reaction kettle. According to the reduction-condensation combined reaction device, the reduction reaction and the condensation reaction are carried out in the same equipment, the distillation procedure is reduced, the consumption of raw materials and the consumption of energy are reduced, the condensation measurement steps are simplified, and the reaction feeding ratio is stable.
Description
Technical field
The utility model relates to a kind of association response device, is mainly the reduction condensation association response device that a kind of cumyl peroxide is manufactured.
Background technology
Existing cumyl peroxide mainly makes by the following method, specific as follows: hydrogen phosphide cumene (mass concentration 50% left and right) first reacts with reducing agent, generates α, alpha-alpha-dimethyl benzylalcohol (abbreviation benzylalcohol); Then the benzylalcohol of low concentration, after washing, rectification under vacuum, obtains the benzylalcohol of high concentration; The benzylalcohol of last high concentration reacts with hydrogen phosphide cumene again, and output is cumyl peroxide.
There is following problem in existing technology:
1, reaction process is long, and the energy, spillage of material are large, waste of manpower resource;
2, the benzylalcohol fusing point of high concentration is low, and the situation of line clogging easily occurs in production process;
3, intermittent reaction is many, participates in consersion unit quantity many;
4, reactor temperature control is more difficult, easily blasts;
5, the effect stirring is poor, undercompounding.
Summary of the invention
Goal of the invention: it is long that the purpose of this utility model is to solve existing reaction unit reaction process, the benzylalcohol solubility of high concentration is low, easily there is in process of production pipeline gambling plug, the reaction of course of reaction discontinuous is many, reactor temperature control is more difficult, participates in the problems such as consersion unit quantity is many, and a kind of raw-material waste that reduces is provided, reduce the concentration affects of subsequent production, the reduction condensation association response device of enhancing productivity.
Technical scheme: in order to realize foregoing invention object, the utility model has been taked following technical scheme:
A kind of reduction condensation association response device, comprise vulcanized sodium dissolution kettle, reactor, solution pump, washing discharging pump, condenser, condensation liquid bath, pick trough, sodium sulfide solution pipeline, the import of described vulcanized sodium dissolution kettle is connected with the first water supply pipe, the outlet of described vulcanized sodium dissolution kettle is connected with described sodium sulfide solution pipeline, described sodium sulfide solution pipeline is connected with described solution pump, described solution pump is provided with two outlets, be divided into other return duct and commissioning pipe, described return duct is connected with the import of described vulcanized sodium dissolution kettle, described commissioning pipe is connected with the top inlet of described reactor, the top inlet of described reactor is also connected with respectively the first pipeline, second pipe, the water inlet of described reactor is connected with the 3rd pipeline, described the 3rd pipeline is connected with the outlet of described pick trough, the outlet of described pick trough is connected with the second water supply pipe, the bottom of reactor is provided with discharging opening and air inlet, described discharging opening is connected with the 7th pipeline, described the 7th pipeline is connected with the import of described washing discharging pump and is connected, described air inlet is connected with respectively the 5th pipeline, the 6th pipeline, described the 6th pipeline is provided with sample valve group, the top of described reactor is provided with bleed outlet and vacuum port, described bleed outlet is connected with the 4th pipeline, described vacuum port is connected with vacuum pipe, described vacuum pipe is connected with the sample valve group that described the 6th pipeline is provided with, described vacuum pipe is also connected with the top inlet of described condenser, the top exit of described condenser is connected with the 8th pipeline, described the 8th pipeline is connected with vacuum system, the outlet at bottom of described condenser is connected with the 9th pipeline, the charging aperture of described the 9th pipeline is connected with the import of described condensation liquid bath, described reactor is also provided with perchloric acid charge door.The utility model is by the improvement of reaction unit, the adjustment of the concentration of reaction raw materials, original two intermittent reactions are completed simultaneously in a reaction unit, and reduce the operation of rectifying, simultaneous reactions material ratio is stablized controlled, reduce raw-material waste, reduce the concentration affects of subsequent production, enhance productivity.
The top bleed outlet of described reactor is provided with the rupture disk that malleation 0.05Mpa breaks, the bottom air inlet of described reactor is provided with visor and stop valve, the rupture disk being provided with effectively prevents that product from blasting in course of reaction again, situation by visor in can observing response still, can pass through stop valve, off-response still if there is something special.
Described reactor is provided with coil pipe, chuck, stirring, thermometer, liquid level gauge, and the thermometer being provided with and liquid level gauge can effectively be measured temperature and liquid level.
Described coil pipe is provided with independent refrigerant and heating agent, and described refrigerant and heating agent are equipped with automatic regulating valve, and described chuck is provided with independent heating agent, by the control of heat exchange medium temperature, indirectly controls the temperature of material in reactor, keeps the temperature difference of heat transferring medium and material.
Described the 5th pipeline is provided with automatic regulating valve, and the vertical height of the drain of described the 5th pipeline is greater than the height of described reactor, without manual operation, and the resource of saving.
The charging aperture of described the 9th pipeline inserts below the liquid level of described condensation liquid bath, keeps fluid-tight state, prevents that pollutant from entering, and the vertical height of described the 9th pipeline is greater than 12 meters, effectively defines the height of the 9th pipeline.
Described condensation liquid bath is provided with blow-down pipe and liquid level gauge, described pick trough is provided with blow-down pipe, floater water intaking valve, liquid level, can prevent sleet intrusion and external foreign matters from being blocked blow-down pipe, can automatically discharge condensate water, air and other incondensable gas, and the valve of the steam leakage that blocks water and the effective liquid level of measuring.
Described condenser is provided with independent refrigerant, can better control the temperature of material in reactor.
Described vulcanized sodium dissolution kettle is provided with agitator, liquid level gauge, vulcanized sodium dog-house, conveniently feeds intake, and by stirring, raw material is mixed fully.
Described washing discharging pump is provided with three outlets, is respectively thick condensation liquid pipeline, mother-liquor waterpipe, reduction washings pipeline, makes like this liquid in raw material better be classified,
Operation principle: solid sodium sulfide is after water-soluble solution, sodium sulfide solution enters reactor, hydrogen phosphide cumene enters reactor again, carry out reduction reaction with vulcanized sodium, obtain hydrogen phosphide cumene, benzylalcohol, isopropylbenzene, the mixed liquor of mother-liquor water, get rid of sinking mother-liquor water through precipitation, mother liquor adds in washing kettle, again through oxalic acid washing, liquid caustic soda washing, water washing, impurity layer is removed in layering, add again water washing repeatedly, washings are drained, through the mixing oil reservoir of washing, add perchloric acid as catalyst, carry out condensation reaction, finally obtain product cumyl peroxide.
Beneficial effect: the utility model compared with prior art tool has the following advantages:
1, first by after solid sodium sulfide hydrolysis, sodium sulfide solution and hydrogen phosphide cumene join and in reactor, carry out reduction reaction and add perchloric acid again and carry out condensation as catalysis, reduction reaction and condensation reaction are carried out in same equipment, have reduced the quantity of consersion unit, have improved production efficiency;
2, reduce the distillation process of thick benzylalcohol, reduced the consumption of raw material and the energy, reduced the concentration of subsequent production;
3, reduce the step of condensation metering, reaction ingredient proportion is stable;
4, adopt the cooling method of coil pipe, make temperature controlled, ensure security;
5, by the control of heat exchange medium temperature, indirectly control the temperature of material in reactor, keep the temperature difference of heat transferring medium and material.
Brief description of the drawings
Fig. 1 is structural representation of the present utility model;
In figure: 1-vulcanized sodium dissolution kettle, 2-reactor, 3-solution pump, 4-washs discharging pump, 5-condenser, 6-vacuum system, 7-condensation liquid bath, 8-pick trough, 9-the first water supply pipe, 10-sodium sulfide solution pipeline, 11-return duct, 12-commissioning pipe, 13-the first pipeline, 14-second pipe, 15-perchloric acid charge door, 16-the second water supply pipe, 17-the 3rd pipeline, 18-vacuum pipe, 19-the 4th pipeline, 20-the 5th pipeline, 21-the 6th pipeline, 22-the 7th pipeline, 23-the 8th pipeline, 24-the 9th pipeline.
Detailed description of the invention
Below in conjunction with accompanying drawing and by specific embodiment, the utility model is further elaborated, be noted that for those skilled in the art, do not departing under the prerequisite of the utility model principle, the amendment of the various equivalent form of values of the present utility model is all being fallen within to the application's claims limited range.
Embodiment:
A kind of reduction condensation association response device as shown in Figure 1, comprise vulcanized sodium dissolution kettle 1, reactor 2, solution pump 3, washing discharging pump 4, condenser 5, condensation liquid bath 7, pick trough 8, sodium sulfide solution pipeline 10, the import of described vulcanized sodium dissolution kettle 1 is connected with the first water supply pipe 9, the outlet of described vulcanized sodium dissolution kettle 1 is connected with described sodium sulfide solution pipeline 10, described sodium sulfide solution pipeline 10 is connected with described solution pump 3, described solution pump 3 is provided with two outlets, be divided into other return duct 11 and commissioning pipe 12, described return duct 11 is connected with the import of described vulcanized sodium dissolution kettle 1, described commissioning pipe 12 is connected with the top inlet of described reactor 2, the top inlet of described reactor 2 is also connected with respectively the first pipeline 13, second pipe 14, described second pipe 14 connects hydrogen phosphide cumene, the water inlet of described reactor 2 is connected with the 3rd pipeline 17, described the 3rd pipeline 17 is connected with the outlet of described pick trough 8, the outlet of described pick trough 8 is connected with the second water supply pipe 16, the bottom of reactor 2 is provided with discharging opening and air inlet, described discharging opening is connected with the 7th pipeline 22, outlet divides three, be respectively thick condensation liquid pipeline, mother-liquor waterpipe, reduction washings pipeline, described the 7th pipeline 22 is connected with the import of described washing discharging pump 4 and is connected, described air inlet is connected with respectively the 5th pipeline 20, the 6th pipeline 21, described the 6th pipeline 21 is provided with sample valve group, the top of described reactor 2 is provided with bleed outlet and vacuum port, described bleed outlet is connected with the 4th pipeline 19, described vacuum port is connected with vacuum pipe 18, described vacuum pipe 18 is connected with the sample valve group that described the 6th pipeline 21 is provided with, described vacuum pipe 18 is also connected with the top inlet of described condenser 5, the top exit of described condenser 5 is connected with the 8th pipeline 23, described the 8th pipeline 23 is connected with vacuum system 6, the outlet at bottom of described condenser 5 is connected with the 9th pipeline 24, the charging aperture of described the 9th pipeline 24 is connected with the import of described condensation liquid bath 7, the 9th pipeline 24 inserts below condensation liquid bath 7 liquid levels, keep fluid-tight state, the vertical height of described the 9th pipeline 24 is greater than 12 meters, described reactor 2 is also provided with perchloric acid charge door 15, described hydrogen phosphide cumene is to enter with reactor 2 to be connected by second pipe 14.
Described the 5th pipeline 20 is provided with automatic regulating valve, and the vertical height of the drain of described the 5th pipeline 20 is greater than the height of described reactor 2.
Described condenser 5 is provided with independent refrigerant, and coolant media is ethylene glycol solution.
Described coil pipe is provided with independent refrigerant and heating agent, and coolant media is recirculated water, and thermal medium is superheated steam, and described refrigerant and heating agent are equipped with automatic regulating valve, and described chuck is provided with independent heating agent, and thermal medium is 80 DEG C of hot water.
Described reactor is provided with coil pipe, chuck, stirring, thermometer, liquid level gauge.
Described condensation liquid bath 24 is provided with blow-down pipe and liquid level gauge.
Described pick trough 8 is provided with blow-down pipe, floater water intaking valve, liquid level gauge.
Described vulcanized sodium dissolution kettle 1 is provided with agitator, liquid level gauge, vulcanized sodium dog-house.
The course of work is as follows:
Solid sodium sulfide in the utility model carries out water-soluble solution in vulcanized sodium dissolution kettle 1, obtain the solution of mass concentration 15% left and right, first drop in reactor 2, the hydrogen phosphide cumene of mass concentration 60% left and right, by second pipe 14 again after the metering of mass flowmenter, be added dropwise in reactor 2, carry out reduction reaction with sodium sulfide solution, temperature is controlled at 72 DEG C of left and right, normal pressure, after vulcanized sodium reacts completely, through row's mother-liquor water, after twice washing draining, in reactor 2, drip perchloric acid (mass concentration 48%), mixed liquor is under perchloric acid catalysis, 42 DEG C of left and right of temperature control, pressure control-0.05Mpa left and right, carry out condensation reaction, finally obtain cumyl peroxide product.
The utility model is by the improvement of reaction unit, the adjustment of the concentration of reaction raw materials, original two intermittent reactions are completed simultaneously in a reaction unit, and reduce the operation of rectifying, simultaneous reactions material ratio is stablized controlled, reduce raw-material waste, reduce the concentration affects of subsequent production, enhance productivity, by being provided with agitator in reactor, stirring is fully mixed the material in reactor, adopt acid solution, aqueous slkali, water washs, make the organic impurities in mother liquor, inorganic impurity is all effectively removed, utilize the cooling method of coil pipe, make temperature controlled, ensure security, by the control of heat exchange medium temperature, indirectly control the temperature of material in reactor, keep the temperature difference of heat transferring medium and material.
Claims (10)
1. a reduction condensation association response device, it is characterized in that: comprise vulcanized sodium dissolution kettle (1), reactor (2), solution pump (3), washing discharging pump (4), condenser (5), condensation liquid bath (7), pick trough (8), sodium sulfide solution pipeline (10), the import of described vulcanized sodium dissolution kettle (1) is connected with the first water supply pipe (9), the outlet of described vulcanized sodium dissolution kettle (1) is connected with described sodium sulfide solution pipeline (10), described sodium sulfide solution pipeline (10) is connected with described solution pump (3), described solution pump (3) is provided with two outlets, be divided into other return duct (11) and commissioning pipe (12), described return duct (11) is connected with the import of described vulcanized sodium dissolution kettle (1), described commissioning pipe (12) is connected with the top inlet of described reactor (2), the top inlet of described reactor (2) is also connected with respectively the first pipeline (13), second pipe (14), the water inlet of described reactor (2) is connected with the 3rd pipeline (17), described the 3rd pipeline (17) is connected with the outlet of described pick trough (8), the outlet of described pick trough (8) is connected with the second water supply pipe (16), the bottom of reactor (2) is provided with discharging opening and air inlet, described discharging opening is connected with the 7th pipeline (22), described the 7th pipeline (22) is connected with the import of described washing discharging pump (4) and is connected, described air inlet is connected with respectively the 5th pipeline (20), the 6th pipeline (21), described the 6th pipeline (21) is provided with sample valve group, the top of described reactor (2) is provided with bleed outlet and vacuum port, described bleed outlet is connected with the 4th pipeline (19), described vacuum port is connected with vacuum pipe (18), described vacuum pipe (18) is connected with the sample valve group that described the 6th pipeline (21) is provided with, described vacuum pipe (18) is also connected with the top inlet of described condenser (5), the top exit of described condenser (5) is connected with the 8th pipeline (23), described the 8th pipeline (23) is connected with vacuum system (6), the outlet at bottom of described condenser (5) is connected with the 9th pipeline (24), the charging aperture of described the 9th pipeline (24) is connected with the import of described condensation liquid bath (7), described reactor (2) is also provided with perchloric acid charge door (15).
2. reduction condensation association response device according to claim 1, is characterized in that: the top bleed outlet of described reactor (2) is provided with the rupture disk that malleation 0.05Mpa breaks, the bottom air inlet of described reactor (2) is provided with visor and stop valve.
3. reduction condensation association response device according to claim 1, is characterized in that: described reactor (2) is provided with coil pipe, chuck, stirring, thermometer, liquid level gauge.
4. reduction condensation association response device according to claim 3, is characterized in that: described coil pipe is provided with independent refrigerant and heating agent, and described refrigerant and heating agent are equipped with automatic regulating valve, and described chuck is provided with independent heating agent.
5. reduction condensation association response device according to claim 1, is characterized in that: described the 5th pipeline (20) is provided with automatic regulating valve, and the vertical height of the drain of described the 5th pipeline (20) is greater than the height of described reactor (2).
6. reduction condensation association response device according to claim 1, it is characterized in that: the charging aperture of described the 9th pipeline (24) inserts below the liquid level of described condensation liquid bath (7), keep fluid-tight state, the vertical height of described the 9th pipeline (24) is greater than 12 meters.
7. reduction condensation association response device according to claim 1, is characterized in that: described condensation liquid bath (7) is provided with blow-down pipe and liquid level gauge, described pick trough (8) is provided with blow-down pipe, floater water intaking valve, liquid level.
8. reduction condensation association response device according to claim 1, is characterized in that: described condenser (5) is provided with independent refrigerant.
9. reduction condensation association response device according to claim 1, is characterized in that: described vulcanized sodium dissolution kettle (1) is provided with agitator, liquid level gauge, vulcanized sodium dog-house.
10. reduction condensation association response device according to claim 1, is characterized in that: described washing discharging pump (4) is provided with three outlets, is respectively thick condensation liquid pipeline, mother-liquor waterpipe, reduction washings pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420193355.2U CN203764265U (en) | 2014-04-21 | 2014-04-21 | Reduction-condensation combined reaction device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420193355.2U CN203764265U (en) | 2014-04-21 | 2014-04-21 | Reduction-condensation combined reaction device |
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| CN203764265U true CN203764265U (en) | 2014-08-13 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103933922A (en) * | 2014-04-21 | 2014-07-23 | 太仓塑料助剂厂有限公司 | Reduction and condensation combined reaction device |
| CN110066234A (en) * | 2019-04-01 | 2019-07-30 | 江苏道明化学有限公司 | A kind of DCP reduction reaction process |
-
2014
- 2014-04-21 CN CN201420193355.2U patent/CN203764265U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103933922A (en) * | 2014-04-21 | 2014-07-23 | 太仓塑料助剂厂有限公司 | Reduction and condensation combined reaction device |
| CN103933922B (en) * | 2014-04-21 | 2016-02-24 | 太仓塑料助剂厂有限公司 | A kind of reduction condensation association response device |
| CN110066234A (en) * | 2019-04-01 | 2019-07-30 | 江苏道明化学有限公司 | A kind of DCP reduction reaction process |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140813 Termination date: 20200421 |