CN1294118A - Equipment for refining 2,4-dinitro chlorobenzone and its crystallizing process - Google Patents
Equipment for refining 2,4-dinitro chlorobenzone and its crystallizing process Download PDFInfo
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- CN1294118A CN1294118A CN 99122068 CN99122068A CN1294118A CN 1294118 A CN1294118 A CN 1294118A CN 99122068 CN99122068 CN 99122068 CN 99122068 A CN99122068 A CN 99122068A CN 1294118 A CN1294118 A CN 1294118A
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Abstract
An equipment and process for refining 2,4-dinitro chlorobenzene is disclosed. Said equipment is a horizontal crystallizer containing tens horizontal water-circulating tubes, each linked to water inlet cavity and water outlet cavity. Said proceess includes loading 2,4-dinitro chlorobenzene into said crystallizer, lowering temp to lower than 22 deg.C at speed of 1-2 deg.C per 15 min, keeping the temp, raising temp to 46 deg.C at speed of 1-3 deg.C per 15 min, keeping the temp, measuring the settling point to be higher than 45.6 deg.C, clossing valve, raising temp to 80 deg.C and discharging the molten refined material.
Description
The invention belongs to chemical industry equipment and crystallization processes, relate generally to and a kind ofly be used for 2, the equipment of 4-dinitrochlorobenzene and crystallization processes.
2 of the Ministry of Chemical Industry's regulation, the quality index of 4-dinitrochlorobenzene is divided into premium grads, acceptable end product and salable product to product according to the ctystallizing point of product is different with purity.But both be that premium grads also is difficult to medicine intermediate 2, the production of 4-dinitrofluorobenzene, 2, the 4-dinitrofluorobenzene is the main raw material of antibiosis anti-inflammatory drug " Norxin ", it is mainly produced as raw material by fluorine is stupid, if with 2, the 4-dinitrochlorobenzene substitutes, and the ton cost can reduce by 4000 yuan, but to 2, the specification of quality of 4-dinitrochlorobenzene is very high, ctystallizing point 〉=48.0 ℃, purity 〉=99%.At present, for Benzene Chloride produce 2, equipment that the 4-dinitrochlorobenzene is purified and technology are difficult to reach standard.Because produce 2 in Benzene Chloride, 4-dinitrochlorobenzene (being called for short 2,6 oil) is washed at worker's tail water and is difficult in the process separate, and influences product purity and zero pour.
The purpose of this invention is to provide a kind of be used for refining 2, the equipment of 4-dinitrochlorobenzene and crystallization processes, it makes 2, the purity of 4-dinitrochlorobenzene and ctystallizing point all are higher than top grade product standard promulgated by the ministries or commissions of the Central Government, can satisfy the needs of medicine intermediate.
Purpose of the present invention adopts following technical scheme to realize: adopt horizontal crystallizer, it has a columniform housing, the bottom of housing is provided with two bases, left end at housing is provided with an intake antrum, right-hand member is provided with a water chamber, intake antrum and water chamber and housing inner chamber separate with dividing plate respectively, enclosure interior is provided with the water pipe bracing frame that intermeshes, tens of water circulating pipes are horizontally fixed on the water pipe bracing frame, each root water circulating pipe one end leads to intake antrum, the other end pass-out water cavity, the water chamber bottom picks out the mouth of a river by a pipeline that is arranged on housing inner chamber bottom, be equipped with temperature measurer in the intravital upper and lower of shell, between two bases in the bottom of housing three drain holes be set, the top of housing is provided with opening for feed to look around mouth.
Crystallization processes is: raw material is the one-level 2 that Benzene Chloride is produced, the 4-dinitrochlorobenzene, charging is preceding with filling with 50 ℃ hot water in the horizontal water-circulating pipe of water pump in horizontal crystallizer, charging behind the circulation several minutes, material injects tap water after advancing to expire in water tank, water temperature is since 50 ℃ of coolings, speed was fallen 1-2 ℃ by per 15 minutes, reduce to below 22 ℃, kept 2-3 hour, open the crystallizer bottom, put down by the material of tip-off, in water tank, inject simultaneously an amount of steam, water temperature heated up beginning below 22 ℃, heat up by per 15 minutes 1-3 ℃, rising to 46 ℃ keeps, when the tested wet product zero pour of putting down reaches more than 45.6 ℃, close the crystallizer bottom valve, when again the water temperature of water cycle being risen to 80 ℃ of left and right sides, door is closed in the bottom open, finished product is put into the finished product jar.
Described horizontal crystallizer connects a pipeline at its water outlet place, pipeline go out the height that open height is higher than water-in.The bottom of intake antrum is provided with the dewatering outlet, and top is provided with the water overflow port.
On described horizontal crystallizer internal cavity Lower Half one all inwalls an interlayer being set, is cavity between interlayer and the inwall, and lower housing portion is provided with an interlayer steam inlet and a steam outlet, communicates with the interlayer cavity of housing Lower Half.
Equipment of the present invention and crystallization processes have following advantage: plant capacity is big, and water circulating pipe is horizontally disposed with, and the worker is easy to operate; Material melting crystal, separation, space between nest of tubes is big, effective; Recirculated water is the while split flow in the middle of level pipe, and temperature is convenient to control; Adopt slow heating and cooling technology in the crystallisation process, make 2, the 6-dinitrochlorobenzene is from 2, separate in the 4-dinitrochlorobenzene, 2 after the purification, 4-dinitrochlorobenzene quality index all is higher than top grade product standard promulgated by the ministries or commissions of the Central Government, ctystallizing point 〉=48.8 ℃, purity is 99.0-99.6%, it can substitute fluorobenzene fully and produce medicine intermediate 2, the 4-dichlor fluorbenzene, per ton cost reduces about 4000 yuan, its purified 2, and the 4-dinitrochlorobenzene is continuously to three batches of Japan outlets, totally 54 tons, obtained good evaluation.
The present invention is described in more detail in conjunction with the embodiments.
Fig. 1 is a device structure synoptic diagram of the present invention.
Equipment as shown in the figure comprises a columniform housing 10, housing 10 bottoms are provided with the base 15 that is used to install and fix, left end at housing 10 is provided with an intake antrum 2, right-hand member is provided with a water chamber 13, intake antrum 2 side upper and lower settings have circulation water-in 1 and water outlet 19, intake antrum 2 tops are provided with water overflow port 3, the bottom is provided with dewatering outlet 18, intake antrum 2, water chamber 13 separates with dividing plate respectively with housing 10 inner chambers, housing 10 inside are provided with the water pipe bracing frame 9 that intermeshes, tens of water circulating pipes 11 are horizontally fixed on the water pipe bracing frame 9, each root water circulating pipe one end leads to intake antrum 2, the other end pass-out water cavity 13, water chamber 13 bottoms pick out the mouth of a river 19 by a pipeline that is arranged on housing 10 inner chamber bottoms, upper and lower in housing 10 is equipped with temperature measurer 12, and the top of housing 10 is provided with opening for feed 5 and looks around mouth 6, between two bases 15 in housing 10 bottoms three drain holes 16 is set.19 places connect a pipeline at water outlet, pipeline go out the height that open height is higher than water-in 3.On one all inwalls of housing 10 inner chamber Lower Halves an interlayer is set, forms interlayer chamber 8 between interlayer and the inwall.Interlayer steam inlet 4 and steam outlet 7 on one are set on the housing 10 upper inlet walls, its with the housing inlet wall in the interlayer cavity communicate.The bottom of housing 10 also is provided with steam inlet 17 and steam outlet 14, and its interlayer cavity with housing 10 Lower Halves communicates, and the cavity between interlayer and the housing 10 Lower Half inwalls can fill steam.
The crystallization processes process is: the one-level 2 that raw material is produced with Benzene Chloride, the 4-dinitrochlorobenzene, close the crystallizer bottom valve before the charging, open the charging valve, survey the SP and the pH value of tundish material, use during for neutrality, utilize before the charging in the water-circulating pipe 11 of water pump in crystallizer and fill with 50 ℃ hot water, treat charging behind the hot water circulation several minutes, after material advances to expire, inject tap water to water tank, water temperature is since 50 ℃ of coolings, speed by 15 minutes 1 ℃ reduce to 20 ℃, when the material temperature drop when not having downtrending, kept 2 hours, and during intensification, closed the tap water inlet valve, open the crystallizer bottom valve, put down the material that is melted, in water tank, feed an amount of steam simultaneously, make the water temperature in the intravital water-circulating pipe of shell begin to heat up at 20 ℃, heat up and press 1 ℃ of per minute, keep when rising to 46 ℃, and measure the wet product zero pour of being put, surveyed zero pour once every 15 minutes, when the wet product zero pour of being surveyed reaches 46 ℃, with crystallizer bottom valve Close All, when injecting steam rises to 80 ℃ with water temperature in water pipe, change material, after material in the device to be crystallized all melts, close heavy vapour, the pump of cutting off the water is opened the crystallizer bottom valve, and finished product is put into the finished product jar from drain hole 16.
Claims (4)
1, a kind of being used for makes with extra care 2, the equipment of 4-dinitrochlorobenzene, has a columniform housing (10), housing (10) bottom is provided with base (15), it is characterized in that: the left end at housing (10) is provided with an intake antrum (2), right-hand member is provided with a water chamber (13), intake antrum (2) side upper and lower settings has circulation water-in (1) and water outlet (19), intake antrum (2) and water chamber (13) both and housing (10) inner chamber separate with dividing plate respectively, housing (10) inside is provided with the water pipe bracing frame (9) that intermeshes, tens of water circulating pipes (11) are horizontally fixed on the water pipe bracing frame (9), each root water circulating pipe one end leads to intake antrum (2), the other end pass-out water cavity (13), water chamber (13) bottom is by a pipeline exit (19) that is arranged on housing (10) inner chamber bottom, upper and lower in housing (10) is equipped with temperature measurer (12), the top of housing (10) is provided with opening for feed (5) and looks around mouthful (6), between two bases (15) of housing (10) bottom three drain holes (16) is set.
2, a kind of utilization equipment according to claim 1 is used for refining 2, the crystallization processes of 4-dinitrochlorobenzene, the one-level 2 of charging for producing with Benzene Chloride, the 4-dinitrochlorobenzene, close the crystallization bottom valve before the charging, open the charging valve, survey the SP and the pH value of tundish raw material, use during for neutrality, it is characterized in that: charging is preceding by filling with 50 ℃ hot water in the horizontal water-circulating pipe (11) of water pump in horizontal crystallizer, the laggard material of several minutes to be recycled, after material advances to expire, in water tank, inject tap water, water temperature is since 50 ℃ of coolings, speed was fallen 1-2 ℃ by per 15 minutes and is reduced to below 22 ℃, kept 2-3 hour, open the crystallizer bottom valve, put down the material that is melted, in water tank, inject an amount of steam simultaneously, water temperature is heated up beginning below 22 ℃, heat up by per 15 minutes 1-3 ℃, rise to 46 ℃ and keep, and measure the wet product zero pour put, surveyed zero pour once every 15-30 minute, when being reached more than 45.6 ℃, with crystallizer bottom valve Close All by hygrometric product zero pour, injecting steam in water pipe, material in material when water temperature is risen to 80 ℃ of left and right sides, device to be crystallized closes steam after all melting, the pump of cutting off the water, the crystallizer bottom valve is opened, and finished product is put into the finished product jar from drain hole (16).
3, according to claim 1ly be used for refiningly 2, the equipment of 4-dinitrochlorobenzene is characterized in that: locate to connect a pipeline at crystallizer water outlet (19), pipeline go out the height that open height is higher than water-in (3).
4, according to claim 1 being used for makes with extra care 2, the equipment of 4-dinitrochlorobenzene, it is characterized in that: establish an interlayer on described crystallizer housing inner chamber Lower Half one all inwalls, form cavity (8) between interlayer and the inwall, lower housing portion is provided with an interlayer steam inlet (17) and steam outlet (14), communicates with the interlayer cavity (8) of housing Lower Half.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99122068 CN1294118A (en) | 1999-10-27 | 1999-10-27 | Equipment for refining 2,4-dinitro chlorobenzone and its crystallizing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99122068 CN1294118A (en) | 1999-10-27 | 1999-10-27 | Equipment for refining 2,4-dinitro chlorobenzone and its crystallizing process |
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| Publication Number | Publication Date |
|---|---|
| CN1294118A true CN1294118A (en) | 2001-05-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 99122068 Pending CN1294118A (en) | 1999-10-27 | 1999-10-27 | Equipment for refining 2,4-dinitro chlorobenzone and its crystallizing process |
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| CN (1) | CN1294118A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113582849A (en) * | 2020-04-30 | 2021-11-02 | 浙江省常山长盛化工有限公司 | Method for producing sulfur black based on mixed low oil of physically purified 2, 4-dinitrochlorobenzene |
| CN113582851A (en) * | 2020-04-30 | 2021-11-02 | 浙江省常山长盛化工有限公司 | Method for producing dinitrophenol based on mixed low oil |
| CN115160141A (en) * | 2021-04-01 | 2022-10-11 | 浙江省常山长盛化工有限公司 | Method for producing 2,4-dinitrochlorobenzene by one-step nitration of chlorobenzene |
-
1999
- 1999-10-27 CN CN 99122068 patent/CN1294118A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113582849A (en) * | 2020-04-30 | 2021-11-02 | 浙江省常山长盛化工有限公司 | Method for producing sulfur black based on mixed low oil of physically purified 2, 4-dinitrochlorobenzene |
| CN113582851A (en) * | 2020-04-30 | 2021-11-02 | 浙江省常山长盛化工有限公司 | Method for producing dinitrophenol based on mixed low oil |
| CN115160141A (en) * | 2021-04-01 | 2022-10-11 | 浙江省常山长盛化工有限公司 | Method for producing 2,4-dinitrochlorobenzene by one-step nitration of chlorobenzene |
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