CN109293529A - A kind of purifying plant and method producing Bravo of the hexachloro-benzene no more than 10ppm - Google Patents
A kind of purifying plant and method producing Bravo of the hexachloro-benzene no more than 10ppm Download PDFInfo
- Publication number
- CN109293529A CN109293529A CN201811486502.4A CN201811486502A CN109293529A CN 109293529 A CN109293529 A CN 109293529A CN 201811486502 A CN201811486502 A CN 201811486502A CN 109293529 A CN109293529 A CN 109293529A
- Authority
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- China
- Prior art keywords
- product
- bravo
- kettle
- rectifying
- trap
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- CKAPSXZOOQJIBF-UHFFFAOYSA-N hexachlorobenzene Chemical compound ClC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl CKAPSXZOOQJIBF-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims description 28
- 239000002994 raw material Substances 0.000 claims abstract description 60
- 238000007670 refining Methods 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims description 47
- 230000008018 melting Effects 0.000 claims description 44
- 238000002844 melting Methods 0.000 claims description 44
- 239000003039 volatile agent Substances 0.000 claims description 40
- 229910001220 stainless steel Inorganic materials 0.000 claims description 36
- 238000000746 purification Methods 0.000 claims description 21
- 229910000856 hastalloy Inorganic materials 0.000 claims description 20
- 229910000934 Monel 400 Inorganic materials 0.000 claims description 19
- OANFWJQPUHQWDL-UHFFFAOYSA-N copper iron manganese nickel Chemical compound [Mn].[Fe].[Ni].[Cu] OANFWJQPUHQWDL-UHFFFAOYSA-N 0.000 claims description 19
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 8
- 239000010962 carbon steel Substances 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 4
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000010924 continuous production Methods 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 120
- 239000007787 solid Substances 0.000 description 11
- 108010066057 cabin-1 Proteins 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 241000894006 Bacteria Species 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000000843 powder Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 239000000155 melt Substances 0.000 description 3
- 239000002910 solid waste Substances 0.000 description 3
- XCJXQCUJXDUNDN-UHFFFAOYSA-N chlordene Chemical compound C12C=CCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl XCJXQCUJXDUNDN-UHFFFAOYSA-N 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 208000031888 Mycoses Diseases 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
Abstract
The present invention relates to a kind of purifying plants and method for producing Bravo of the hexachloro-benzene no more than 10ppm, and the purifying plant includes sequentially connected raw material feed unit, purifier units and product collector unit；The purifier units include rectifying column, refining kettle and condenser, and the tower bottom discharge port of rectifying column and the feed inlet of refining kettle connect, and the discharge port of refining kettle and the feed inlet of condenser connect.Rectifying column and refining kettle are combined by the present invention, the Bravo that hexachlorobenzene content is 10-100ppm is reused rectifying still after rectifying column rectifying to refine, reduce the hexachlorobenzene content in Bravo, the content of hexachloro-benzene in Bravo product is set to be no more than 10ppm, the content of Bravo can be to 99.7% in Bravo product, and purifying plant provided by the invention can carry out continuous production, and operating cost is low.
Description
Technical field
The invention belongs to field of pesticide production, are related to a kind of purifying plant more particularly to a kind of purification for producing Bravo
Apparatus and method, in particular to a kind of purifying plant and method for producing Bravo of the hexachloro-benzene no more than 10ppm.
Background technique
Bravo is a kind of efficient, low toxicity, wide spectrum, and the protective fungicide of low-residual is widely used in agricultural and woods
The fungal disease of industry is prevented and treated, using many especially on vegetables, the industrial crops such as fruit.It can be right according to Japanese data report Bravo
52 kinds of diseases of 30 various crops have control efficiency.In addition, Bravo also has important use in mould proof industrial circle,
Such as manufacture mildew resistant paint, mould proof wallpaper, electric appliance is mould proof, Pi Ping, timber etc. it is mould proof.The production scale of Bravo at home is continuous
Expand, it has also become one of excellent pesticide species of large-tonnage in the world.Sale in the international market is constantly in fast-selling situation.Hundred
It is white powder that bacterium defines clearly its appearance in the standard GB/T in China/T 9551-2017, and two main indicators are Bravo
Content >=97wt.%, hexachlorobenzene content≤40ppm are qualified product.International market requires to have to Bravo inherent quality at present
It is apparent to improve, other than content and appearance, especially emphasize that the control to harmful substance HCB (hexachloro-benzene) has higher want
It asks, hexachloro-benzene is not degradable, serious to environmental hazard.International market requires its content to be no more than 10ppm, develops hexachlorobenzene content
Bravo product no more than 10ppm, one seize international market, secondly reducing the harm to environment, therefore produce chlordene
Bravo of the benzene content no more than 10ppm has great importance.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of production hexachloro-benzene to be no more than 10ppm
Bravo purifying plant and method, the purifying plant mentions Bravo by the combination of rectifying column and refining kettle
It is pure, make hexachloro-benzene in Bravo content be no more than 10ppm, and the purifying plant can continuous production, high production efficiency.
To achieve this purpose, the present invention adopts the following technical scheme:
In a first aspect, the present invention provides a kind of purifying plant for producing Bravo of the hexachloro-benzene no more than 10ppm, it is described
Purifying plant includes sequentially connected raw material feed unit, purifier units and product collector unit.
The purifier units include rectifying column, refining kettle and condenser, the tower bottom discharge port of rectifying column and refining kettle into
Material mouth connection, the discharge port of refining kettle and the feed inlet of condenser connect.
The present invention carries out refinement treatment by tower bottom product of the setting refining kettle to rectifying column, and rectifying tower bottom product is hundred
Bacterium is clear, the mixture of hexachloro-benzene and other heavy constituents, carries out refinement treatment to mixture, can obtain hexachlorobenzene content and not surpass
Cross the Bravo product of 10ppm.The purifying plant that the present invention uses is simple, and equipment investment is low, contained in gained Bravo
Hexachlorobenzene content is low.
Preferably, the material of the rectifying column includes any one in 304 stainless steels, Monel 400 or Hastelloy.
Preferably, the rectifying column outer wall is provided with heat tracing pipe.The setting of heat tracing pipe ensure that temperature inside rectifying tower
Stability.
Preferably, described the top of the distillation column is provided with shell and tube condenser.
Preferably, the rectifying tower bottom is provided with shell and tube reboiler.
Preferably, the material of the refining kettle includes any one in 304 stainless steels, Monel 400 or Hastelloy.
Preferably, the outer wall of the refining kettle is provided with collet.It is 260-350 DEG C that temperature is passed through in the collet of refining kettle
Conduction oil, conduction oil heats material in kettle.
Preferably, coil pipe is provided in the kettle of the refining kettle.It is 260-350 DEG C that temperature is passed through in the coil pipe of refining kettle
Conduction oil, conduction oil heats material in kettle.
Preferably, the refining kettle is provided with mechanical stirring.Churned mechanically setting can make the material in refining kettle by
It is hot uniform.
Preferably, the material of the condenser includes any one in 304 stainless steels, Monel 400 or Hastelloy.
Preferably, the condenser is tubular heat exchanger.The tubular heat exchanger uses temperature for 240-330 DEG C
Conduction oil carry out it is thermally conductive.
Preferably, the raw material feed unit include sequentially connected raw material cabin, melting kettle, piping filter, metering pump,
Melting medial launder and superheater, the discharge port of the superheater are connect with the feed inlet of the rectifying column.
Preferably, the material of the raw material cabin includes carbon steel and/or 304 stainless steels.
Preferably, the material of the melting kettle includes any one in 304 stainless steels, Monel 400 or Hastelloy.
Preferably, the outer wall of the melting kettle is provided with collet.It is 260-350 DEG C that temperature is passed through in the collet of melting kettle
Conduction oil, conduction oil carries out heating fusing to material in kettle.
Preferably, the material of the piping filter includes any in 304 stainless steels, Monel 400 or Hastelloy
It is a kind of.
Preferably, the material of the melting medial launder includes any in 304 stainless steels, Monel 400 or Hastelloy
It is a kind of.
Preferably, the outer wall of the melting medial launder is provided with collet.Being passed through temperature in the collet of melting medial launder is
260-350 DEG C of conduction oil, conduction oil carry out heating fusing to material in slot.
Preferably, the material of the superheater includes any one in 304 stainless steels, Monel 400 or Hastelloy.
Preferably, the superheater is tubular heat exchanger.The material being passed through by melting medial launder is heated to by superheater
The bubble point of material.
Preferably, the material of the metering pump includes any one in 304 stainless steels, Monel 400 or Hastelloy.
Preferably, the metering pump includes plunger type metering pump and/or diaphragm metering pump.
Preferably, the product collector unit includes that product receives kettle, product trapping device and product vacuum pump, the production
The feed inlet that product receive kettle is connect with the discharge port of the condenser, and product receives overhead vapor outlet and the product trapping device of kettle
Feeding inlet connection, the gas vent of product trapping device connect with product vacuum pump.
Preferably, the material that the product receives kettle includes any in 304 stainless steels, Monel 400 or Hastelloy
It is a kind of.
Preferably, the outer wall that the product receives kettle is provided with collet.Being passed through temperature in the collet of product reception kettle is
240-330 DEG C of conduction oil, conduction oil heat material in kettle.
Preferably, the material of the product trapping device includes carbon steel and/or 304 stainless steels.
Preferably, the outer wall of the product trapping device is provided with collet.It is 40- that temperature is passed through in the collet of product trapping device
150 DEG C of water or cold air.
Preferably, it is provided with plate washer in the product trapping device, product trapping device is divided into two Room by the plate washer.It is entrained with
The gas of solid particle is after plate washer water conservancy diversion, and solids particles precipitate is in the bottom of product trapping device, wherein the solid particle of deposition
It can be used as qualified products.
Preferably, the product vacuum pump includes appointing in water-ring vacuum pump, piston type vacuum pump or Roots vaccum pump
It anticipates one kind.
Preferably, the purifier units are additionally provided with front-end volatiles trap and front-end volatiles vacuum pump, and the front-end volatiles are caught
Storage is used to trap the light component of the top of the distillation column output, the gas vent company of the front-end volatiles vacuum pump and front-end volatiles trap
It connects.
The solid powder trapped in front-end volatiles trap accounts for about the 1wt% of Bravo feedstock amount, is solid waste, receives
It is focused on after collection.
Preferably, the material of the front-end volatiles trap includes carbon steel and/or 304 stainless steels.
Preferably, the outer wall of the front-end volatiles trap is provided with collet.Temperature is passed through in the collet of front-end volatiles trap
For 40-150 DEG C of water or cold air.
Preferably, it is provided with plate washer in the front-end volatiles trap, front-end volatiles trap is divided into two Room by the plate washer.It is molten
Change in the gas that furnace generates entrained solid particle after plate washer water conservancy diversion, solids particles precipitate in the bottom of front-end volatiles trap,
These solid particles are solid waste, are focused on after collection.
Preferably, the gas outlet of the front-end volatiles trap is provided with filter screen.
Preferably, the front-end volatiles vacuum pump includes in water-ring vacuum pump, piston type vacuum pump or Roots vaccum pump
Any one.
Preferably, the product trapping device includes sequentially connected product trapping device A, product trapping device B and product vacuum
Pump, the gas vent of the product trapping device A are connect with the gas access of the product trapping device B.
Preferably, the raw material feed unit is additionally provided with fusing trap, and the fusing trap is melted with described respectively
Change kettle and melts the gas vent connection of medial launder.
Preferably, the material of the fusing trap includes carbon steel and/or 304 stainless steels.
Preferably, the outer wall of the fusing trap is provided with collet.It is 40- that temperature is passed through in fusing trap collet
150 DEG C of water or cold air.
Preferably, it is provided with plate washer in the fusing trap, front-end volatiles trap is divided into two Room by the plate washer.
Preferably, the gas outlet of the fusing trap is provided with filter screen.
Preferably, the melting kettle, piping filter, metering pump, melting medial launder, superheater, rectifying column, refining kettle,
The connecting line that condenser and product receive between kettle is jacketed piping.Admittance hot oil is in jacketed piping to control in pipeline
The stability of temperature of charge.
Preferably, the material of the jacketed piping includes any one in 304 stainless steels, Monel 400 or Hastelloy
Kind.
Second aspect, the present invention provides a kind of method of purifying plant purification Bravo as described in relation to the first aspect,
It is characterized in that, described method includes following steps:
(1) Bravo raw material is melted, the Bravo after fusing is heated to bubble point；
(2) rectifying is heated to the Bravo of bubble point, carries out refinement treatment to rectifying tower bottom product, traps product, obtain six
Chlorobenzene is no more than the Bravo of 10ppm.
Preferably, Bravo content is 90-99.5wt.% in step (1) the Bravo raw material, such as be can be
90wt.%, 91wt.%, 92wt.%, 93wt.%, 94wt.%, 95wt.%, 96wt.%, 97wt.%, 98wt.%,
99wt.% or 99.5wt.%, preferably 95-99wt.%.
Preferably, in the Bravo raw material hexachlorobenzene content be 10-100ppm, such as can be 10ppm, 20ppm,
30ppm, 40ppm, 50ppm, 60ppm, 70ppm, 80ppm, 90ppm or 100ppm, preferably 30-80ppm.
Preferably, the temperature of the fusing be 260-350 DEG C, such as can be 260 DEG C, 270 DEG C, 280 DEG C, 290 DEG C,
300 DEG C, 310 DEG C, 320 DEG C, 330 DEG C, 340 DEG C or 350 DEG C, preferably 300-330 DEG C.
Preferably, the bubble point temperature is 260-350 DEG C, such as can be 260 DEG C, 270 DEG C, 280 DEG C, 290 DEG C, 300
DEG C, 310 DEG C, 320 DEG C, 330 DEG C, 340 DEG C or 350 DEG C, preferably 300-330 DEG C；
Preferably, the stripping section temperature of step (2) described rectifying be 300-350 DEG C, such as can be 300 DEG C, 310 DEG C,
320 DEG C, 330 DEG C, 340 DEG C or 350 DEG C, preferably 320-330 DEG C.
Preferably, the rectifying section temperature of the rectifying be 260-330 DEG C, such as can be 260 DEG C, 270 DEG C, 280 DEG C,
290 DEG C, 300 DEG C, 310 DEG C, 320 DEG C or 330 DEG C, preferably 280-300 DEG C.
Preferably, the tower top absolute vacuum degree of the rectifying be 0.05-0.095MPa, such as can be 0.05MPa,
0.01MPa, 0.02MPa, 0.03MPa, 0.04MPa, 0.05MPa, 0.06MPa, 0.07MPa, 0.08MPa or 0.095MPa, it is excellent
It is selected as 0.06-0.08MPa.
Preferably, the overhead condenser temperature of the rectifying is 250-330 DEG C, such as can be 250 DEG C, 260 DEG C, 270
DEG C, 280 DEG C, 290 DEG C, 300 DEG C, 310 DEG C, 320 DEG C or 330 DEG C, preferably 260-290 DEG C.
Preferably, the tower bottom reboiler temperature of the rectifying is 300-350 DEG C, such as can be 300 DEG C, 310 DEG C, 320
DEG C, 330 DEG C, 340 DEG C or 350 DEG C, preferably 310-330 DEG C.
Preferably, the temperature of the refinement treatment is 260-350 DEG C, such as can be 260 DEG C, 270 DEG C, 280 DEG C, 290
DEG C, 300 DEG C, 310 DEG C, 320 DEG C, 330 DEG C, 340 DEG C or 350 DEG C, preferably 300-330 DEG C.
Preferably, the vacuum degree of the refinement treatment be 0.05-0.095MPa, such as can be 0.05MPa,
0.01MPa, 0.02MPa, 0.03MPa, 0.04MPa, 0.05MPa, 0.06MPa, 0.07MPa, 0.08MPa or 0.095MPa, it is excellent
It is selected as 0.06-0.08MPa.
Preferably, the temperature of the trapping be 40-150 DEG C, such as can be 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C,
90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C, 130 DEG C, 140 DEG C or 150 DEG C, preferably 60-80 DEG C.
As the optimal technical scheme of second aspect of the present invention providing method, described method includes following steps:
(1) 260-350 DEG C of fusing hexachlorobenzene content is 10-100ppm Bravo raw material, and is heated to 260-350 DEG C
Bubble point temperature；
(2) rectifying is heated to the Bravo of bubble point, and stripping section temperature is 300-350 DEG C, and rectifying section temperature is 260-330
DEG C, the tower top absolute vacuum degree of rectifying is 0.05-0.095MPa, and overhead condenser temperature is 250-330 DEG C, tower bottom reboiler
Temperature is 300-350 DEG C, carries out refinement treatment to tower bottom product, and the temperature of refinement treatment is 260-350 DEG C, refinement treatment it is true
Reciprocal of duty cycle is 0.05-0.095MPa, and 40-150 DEG C traps the product after purification, obtains hexachloro-benzene is no more than 10ppm hundred
The clear product of bacterium.
Numberical range of the present invention not only includes enumerated point value, further includes the above-mentioned numerical value not included
Arbitrary point value between range, as space is limited and for concise consideration, range described in the present invention no longer exclusive list includes
Specific point value.
Compared with prior art, the invention has the benefit that
Rectifying column and refining kettle are combined by the present invention, and the Bravo that hexachlorobenzene content is 10-100ppm is passed through essence
It evaporates and reuses rectifying still after tower rectifying and refined, reduce the hexachlorobenzene content in Bravo, make chlordene in Bravo product
The content of benzene is no more than 10ppm, and the content of Bravo can be to 99.7% in Bravo product, and purification provided by the invention
Device can carry out continuous production, and operating cost is low.
Detailed description of the invention
Fig. 1 is the purifying plant schematic diagram that the embodiment of the present invention 2 provides.
Wherein: 1, raw material cabin；2, screw conveyor；3, melting kettle；4, piping filter；5, plunger type metering pump；6, it melts
Melt medial launder；7, superheater；8, rectifying column；9, refining kettle；10, condenser；11, product receives kettle；12, melt trap；
13, front-end volatiles trap；14, product trapping device A；15, product trapping device B；16, front-end volatiles vacuum pump；17, product vacuum
Pump.
Specific embodiment
To further illustrate the technical scheme of the present invention below with reference to the accompanying drawings and specific embodiments.
I) purifying plant
Embodiment 1
Present embodiments provide a kind of purifying plant for producing Bravo of the hexachloro-benzene no more than 10ppm, the purification dress
It sets including sequentially connected raw material feed unit, purifier units and product collector unit.
The purifier units include rectifying column 8, refining kettle 9 and condenser 10, the tower bottom discharge port and refining kettle of rectifying column 8
9 feed inlet connection, the discharge port of refining kettle 9 connect with the feed inlet of condenser 10, the rectifying column 8, refining kettle 9 and cold
The material of condenser 10 is 304 stainless steels, and the outer wall of the rectifying column 8 is provided with heat tracing pipe, and 8 tower top of rectifying column is provided with shell and tube
Condenser 10,8 tower bottom of rectifying column are provided with shell and tube reboiler, and the outer wall of refining kettle 9 is provided with collet, in the kettle of refining kettle 9
It is provided with coil pipe and mechanical stirring, the condenser 10 is tubular heat exchanger.
The raw material feed unit includes sequentially connected raw material cabin 1, screw conveyor 2, melting kettle 3, piping filter
4, plunger type metering pump 5, melting medial launder 6 and superheater 7, the charging of the discharge port of the superheater 7 and the rectifying column 8
Mouth connection.The raw material cabin 1, melting kettle 3, piping filter 4, plunger type metering pump 5, melting medial launder 6 and superheater 7
Material is 304 stainless steels, and the outer wall of the melting kettle 3 is provided with collet, and the outer wall of melting medial launder 6 is provided with collet, overheats
Device 7 is tubular heat exchanger.
The product collector unit include include product receive kettle 11, product trapping device A14, product trapping device B15 and
Piston type vacuum pump, the feed inlet that the product receives kettle 11 are connect with the discharge port of the condenser 10, and product receives kettle 11
Overhead vapor outlet connect with the feeding inlet of product trapping device, the gas vent of product trapping device and the company of product vacuum pump 17
It connects, the material that product receives kettle 11, product trapping device A14 and product trapping device B15 is 304 stainless steels, and product receives kettle 11
Outer wall be provided with collet, the outer wall of product trapping device A14 and product trapping device B15 are provided with collet, set in product trapping device
It is equipped with plate washer, product trapping device is divided into two Room by the plate washer.
The melting kettle 3, piping filter 4, plunger type metering pump 5, melting medial launder 6, superheater 7, rectifying column 8, essence
The connecting line that kettle 9, condenser 10 and product processed receive between kettle 11 is jacketed piping, the material packet of the jacketed piping
Include 304 stainless steels.
Bravo raw material is continuously conveyed by raw material cabin 1 and screw conveyor 2 to melting kettle 3, and Bravo raw material is molten
Change in kettle 3 and be fused into liquid, is filtered out by piping filter 4 and be continuously conveyed by plunger type metering pump 5 into melting after impurity
Between slot 6, continuously enter rectifying column 8 from the middle part of rectifying column 8 after superheater 7 is heated to bubble point temperature, hexachlorobenzene content compared with
For high light component by tower top output, the Bravo of initial gross separation hexachloro-benzene flows into refining kettle 9, and is evaporated to gas in refining kettle 9
State flows into product after the condensation of condenser 10 and receives kettle 11, and the gas that failed to condensation is in product trapping device A14 and product trapping
Condensation in device B15, the solid that product receives in kettle 11, product trapping device A14 and product trapping device B15 is qualified products.
Embodiment 2
Present embodiments provide a kind of purifying plant for producing Bravo of the hexachloro-benzene no more than 10ppm, the purification dress
The schematic diagram set is as shown in Figure 1, the purifying plant includes that sequentially connected raw material feed unit, purifier units and product are received
Collect unit.
The purifier units include rectifying column 8, refining kettle 9, condenser 10, front-end volatiles trap 13 and front-end volatiles vacuum
Pump 16, the tower bottom discharge port of rectifying column 8 is connect with the feed inlet of refining kettle 9, the discharge port of refining kettle 9 and condenser 10 into
Material mouth connection, the rectifying column 8, refining kettle 9, front-end volatiles trap 13 and condenser 10 material be 304 stainless steels, institute
The outer wall for stating rectifying column 8 is provided with heat tracing pipe, and 8 tower top of rectifying column is provided with shell and tube condenser 10, and 8 tower bottom of rectifying column is provided with
Shell and tube reboiler, the outer wall of refining kettle 9 are provided with collet, and coil pipe and mechanical stirring are provided in the kettle of refining kettle 9, described cold
Condenser 10 is tubular heat exchanger, and the front-end volatiles trap 13 is used to trap the light component of 8 tower top output of rectifying column, described
Front-end volatiles vacuum pump 16 is connect with the gas vent of front-end volatiles trap 13, and the outer wall of front-end volatiles trap 13 is provided with collet,
It is provided with plate washer in front-end volatiles trap 13, front-end volatiles trap 13 is divided to for two Room by the plate washer, front-end volatiles trap 13
Gas outlet is provided with filter screen, and the front-end volatiles vacuum pump 16 is water-ring vacuum pump.
The raw material feed unit includes sequentially connected raw material cabin 1, screw conveyor 2, melting kettle 3, piping filter
4, plunger type metering pump 5, melting medial launder 6, fusing trap 12 and superheater 7, the discharge port of the superheater 7 with it is described
The feed inlet of rectifying column 8 connects.The raw material cabin 1, melting kettle 3, piping filter 4, plunger type metering pump 5, melting medial launder
6, the material for melting trap 12 and superheater 7 is 304 stainless steels, and the outer wall of the melting kettle 3 is provided with collet, in melting
Between the outer wall of slot 6 be provided with collet, superheater 7 is tubular heat exchanger, and the outer wall of fusing trap 12 is provided with collet, melts
It is provided with plate washer in trap 12, the plate washer will melt trap 12 and be divided to for two Room, and the gas of the fusing trap 12 goes out
Filter screen is provided at mouthful.
The product collector unit include include product receive kettle 11, product trapping device A14, product trapping device B15 and
Product vacuum pump 17, the feed inlet that the product receives kettle 11 are connect with the discharge port of the condenser 10, and product receives kettle 11
Overhead vapor outlet connect with the feeding inlet of product trapping device A14, the gas vent of product trapping device and product vacuum pump 17
Connection, the material that product receives kettle 11, product trapping device A14 and product trapping device B15 is 304 stainless steels, and product receives kettle
11 outer wall is provided with collet, and the outer wall of product trapping device A14 and product trapping device B15 are provided with collet, in product trapping device
It is provided with plate washer, product trapping device is divided into two Room by the plate washer.
The melting kettle 3, piping filter 4, plunger type metering pump 5, melting medial launder 6, superheater 7, rectifying column 8, essence
The connecting line that kettle 9, condenser 10 and product processed receive between kettle 11 is jacketed piping, the material packet of the jacketed piping
Include 304 stainless steels.
Bravo raw material is continuously conveyed by raw material cabin 1 and screw conveyor 2 to melting kettle 3, and Bravo raw material is molten
Change in kettle 3 and be fused into liquid, is filtered out by piping filter 4 and be continuously conveyed by plunger type metering pump 5 into melting after impurity
Between slot 6, continuously enter rectifying column 8 from the middle part of rectifying column 8 after superheater 7 is heated to bubble point temperature, hexachlorobenzene content compared with
For high light component by tower top output, the Bravo of initial gross separation hexachloro-benzene flows into refining kettle 9, and is evaporated to gas in refining kettle 9
State flows into product after the condensation of condenser 10 and receives kettle 11, and the gas that failed to condensation is in product trapping device A14 and product trapping
Condensation in device B15, the solid that product receives in kettle 11, product trapping device A14 and product trapping device B15 is qualified products.
The gas generated in melting kettle 3 enters fusing trap 12, and the solid powder melted in trap 12 can be used as hundred
The clear raw material of bacterium is back to raw material cabin 1；8 tower top of rectifying column produces gas and enters front-end volatiles trap 13, consolidating in front-end volatiles trap 13
Body powder is solid waste, does fixed-end forces after concentration.
Comparative example 1
This comparative example provides a kind of purifying plant of Bravo, compared with Example 1, the purification list that this comparative example provides
It is not provided with refining kettle in member, rectifying tower bottom product is transformed into solid and produces directly through collecting after condenser in product in kettle
Product.
II) method of purification
Application examples 1
The application example provides a kind of method of purifying plant purification Bravo raw material using embodiment 2, the method
Include the following steps:
(1) 300 DEG C of fusing hexachlorobenzene content is 60ppm Bravo raw material, and is heated to bubble point temperature, in Bravo raw material
Bravo content is 95wt.%；
(2) rectifying is heated to the Bravo of bubble point, and stripping section temperature is 330 DEG C, and rectifying section temperature is 300 DEG C, rectifying
Tower top absolute vacuum degree is 0.08MPa, and overhead condenser temperature is 290 DEG C, and tower bottom reboiler temperature is 330 DEG C, is produced to tower bottom
Object carries out refinement treatment, and the temperature of refinement treatment is 330 DEG C, and the absolute vacuum degree of refinement treatment is 0.07MPa, and 80 DEG C to purification
Product afterwards is trapped, and the Bravo product that hexachloro-benzene is 6ppm is obtained.
Application examples 2
The application example provides a kind of method of purifying plant purification Bravo raw material using embodiment 2, the method
Include the following steps:
(1) 280 DEG C of fusing hexachlorobenzene content is 40ppm Bravo raw material, and is heated to bubble point temperature, in Bravo raw material
Bravo content is 92wt.%；
(2) rectifying is heated to the Bravo of bubble point, and stripping section temperature is 320 DEG C, and rectifying section temperature is 280 DEG C, rectifying
Tower top absolute vacuum degree is 0.06MPa, and overhead condenser temperature is 260 DEG C, and tower bottom reboiler temperature is 310 DEG C, is produced to tower bottom
Object carries out refinement treatment, and the temperature of refinement treatment is 300 DEG C, and the absolute vacuum degree of refinement treatment is 0.06MPa, and 60 DEG C to purification
Product afterwards is trapped, and the Bravo product that hexachloro-benzene is 5ppm is obtained.
Application examples 3
The application example provides a kind of method of purifying plant purification Bravo raw material using embodiment 2, the method
Include the following steps:
(1) 350 DEG C of fusing hexachlorobenzene content is 100ppm Bravo raw material, and is heated to bubble point temperature, Bravo raw material
Middle Bravo content is 99wt.%；
(2) rectifying is heated to the Bravo of bubble point, and stripping section temperature is 350 DEG C, and rectifying section temperature is 330 DEG C, rectifying
Tower top absolute vacuum degree is 0.095MPa, and overhead condenser temperature is 330 DEG C, and tower bottom reboiler temperature is 350 DEG C, is produced to tower bottom
Object carries out refinement treatment, and the temperature of refinement treatment is 350 DEG C, and the absolute vacuum degree of refinement treatment is 0.05MPa, and 150 DEG C to essence
Product after system is trapped, and the Bravo product that hexachloro-benzene is 10ppm is obtained.
Application examples 4
The application example provides a kind of method of purifying plant purification Bravo raw material using embodiment 2, the method
Include the following steps:
(1) 260 DEG C of fusing hexachlorobenzene content is 10ppm Bravo raw material, and is heated to bubble point temperature, in Bravo raw material
Bravo content is 90wt.%；
(2) rectifying is heated to the Bravo of bubble point, and stripping section temperature is 300 DEG C, and rectifying section temperature is 260 DEG C, rectifying
Tower top absolute vacuum degree is 0.05MPa, and overhead condenser temperature is 250 DEG C, and tower bottom reboiler temperature is 300 DEG C, is produced to tower bottom
Object carries out refinement treatment, and the temperature of refinement treatment is 260 DEG C, and the absolute vacuum degree of refinement treatment is 0.095MPa, and 40 DEG C to essence
Product after system is trapped, and the Bravo product that hexachloro-benzene is 2ppm is obtained.
Application examples 5
The application example provides a kind of method of purifying plant purification Bravo raw material using embodiment 1, the method
Include the following steps:
(1) 300 DEG C of fusing hexachlorobenzene content is 60ppm Bravo raw material, and is heated to bubble point temperature, in Bravo raw material
Bravo content is 95wt.%；
(2) rectifying is heated to the Bravo of bubble point, and stripping section temperature is 330 DEG C, and rectifying section temperature is 300 DEG C, rectifying
Tower top absolute vacuum degree is 0.08MPa, and overhead condenser temperature is 290 DEG C, and tower bottom reboiler temperature is 330 DEG C, is produced to tower bottom
Object carries out refinement treatment, and the temperature of refinement treatment is 330 DEG C, and the absolute vacuum degree of refinement treatment is 0.07MPa, and 80 DEG C to purification
Product afterwards is trapped, and the Bravo product that hexachloro-benzene is 6ppm is obtained.
Comparison study example 1
This application comparative example provides a kind of method of purifying plant purification Bravo raw material using comparative example 1, described
Method includes the following steps:
(1) 300 DEG C of fusing hexachlorobenzene content is 60ppm Bravo raw material, and is heated to bubble point temperature, in Bravo raw material
Bravo content is 95wt.%；
(2) rectifying is heated to the Bravo of bubble point, and stripping section temperature is 330 DEG C, and rectifying section temperature is 300 DEG C, rectifying
Tower top absolute vacuum degree is 0.08MPa, and overhead condenser temperature is 290 DEG C, and tower bottom reboiler temperature is 330 DEG C, and 80 DEG C to tower
Bottom product is cooled down, and the Bravo product that hexachloro-benzene is 15ppm is obtained.
Bravo raw material is handled in application examples 1-5 provided by the invention and Comparison study example 1, to gained Bravo product
And the Bravo rate of recovery is analyzed, the results are shown in Table 1 for analysis:
Table 1
By application examples 1-4 it is found that being purified using method of purification provided by the invention to Bravo raw material, after purification
The content of Bravo is 99.4~99.7wt% in Bravo product, and the content of hexachloro-benzene is 2-10ppm, the rate of recovery of Bravo
For 98.1~98.9wt%.
Purifying plant used in application examples 5 is provided by embodiment 1, and fusing trap is not provided in embodiment 1, can not be to molten
The Bravo raw material for changing tail gas entrainment is recycled, therefore the rate of recovery of Bravo is 96.8wt% in application examples 5, lower than application
The rate of recovery 98.6wt% of Bravo in example 1.
Purifying plant used is provided by comparative example 1 in comparison application examples 1, and refining kettle, rectifying column are not provided in comparative example 1
Bottom product after supercooling up to Bravo product, since rectifying tower bottom product does not pass through the refinement treatment for the treatment of column, hundred
The content of Bravo is reduced to 99.2% by 99.6wt% in the clear product of bacterium, and hexachlorobenzene content rises to 15ppm by 6ppm.
To sum up, rectifying column and refining kettle are combined by the present invention, and the Bravo that hexachlorobenzene content is 10-100ppm is passed through
It crosses after rectifying column rectifying and reuses rectifying still and refined, reduce the hexachlorobenzene content in Bravo, make in Bravo product
The content of hexachloro-benzene is no more than 10ppm, and the content of Bravo can be to 99.7% in Bravo product, and provided by the invention mentions
Pure device can carry out continuous production, and operating cost is low.
The Applicant declares that the foregoing is merely a specific embodiment of the invention, but protection scope of the present invention not office
It is limited to this, it should be clear to those skilled in the art, any to belong to those skilled in the art and take off in the present invention
In the technical scope of dew, any changes or substitutions that can be easily thought of, and all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of purifying plant for producing Bravo of the hexachloro-benzene no more than 10ppm, which is characterized in that the purifying plant includes
Sequentially connected raw material feed unit, purifier units and product collector unit；
The purifier units include rectifying column, refining kettle and condenser, the tower bottom discharge port of rectifying column and the feed inlet of refining kettle
Connection, the discharge port of refining kettle and the feed inlet of condenser connect.
2. purifying plant according to claim 1, which is characterized in that the material of the rectifying column includes 304 stainless steels, covers
Like this 400 or Hastelloy in any one；
Preferably, the rectifying column outer wall is provided with heat tracing pipe；
Preferably, described the top of the distillation column is provided with shell and tube condenser；
Preferably, the rectifying tower bottom is provided with shell and tube reboiler；
Preferably, the material of the refining kettle includes any one in 304 stainless steels, Monel 400 or Hastelloy；
Preferably, the outer wall of the refining kettle is provided with collet；
Preferably, coil pipe is provided in the kettle of the refining kettle；
Preferably, the refining kettle is provided with mechanical stirring；
Preferably, the material of the condenser includes any one in 304 stainless steels, Monel 400 or Hastelloy；
Preferably, the condenser is tubular heat exchanger.
3. purifying plant according to claim 1 or 2, which is characterized in that the raw material feed unit includes being sequentially connected
Raw material cabin, raw material conveying device, melting kettle, piping filter, metering pump, melting medial launder and superheater, the overheat
The discharge port of device is connect with the feed inlet of the rectifying column；
Preferably, the material of the raw material cabin includes carbon steel and/or 304 stainless steels；
Preferably, the raw material conveying device includes conveyer belt and/or screw conveyor；
Preferably, the material of the melting kettle includes any one in 304 stainless steels, Monel 400 or Hastelloy；
Preferably, the outer wall of the melting kettle is provided with collet；
Preferably, the material of the piping filter includes any one in 304 stainless steels, Monel 400 or Hastelloy；
Preferably, the material of the melting medial launder includes any one in 304 stainless steels, Monel 400 or Hastelloy；
Preferably, the outer wall of the melting medial launder is provided with collet；
Preferably, the material of the superheater includes any one in 304 stainless steels, Monel 400 or Hastelloy；
Preferably, the superheater is tubular heat exchanger；
Preferably, the material of the metering pump includes any one in 304 stainless steels, Monel 400 or Hastelloy；
Preferably, the metering pump includes plunger type metering pump and/or diaphragm metering pump；
Preferably, the product collector unit includes that product reception kettle, product trapping device and product vacuum pump, the product connect
The feed inlet for receiving kettle is connect with the discharge port of the condenser, and product receives the overhead vapor outlet of kettle and entering for product trapping device
Material mouth connection, the gas vent of product trapping device are connect with product vacuum pump；
Preferably, it includes any one in 304 stainless steels, Monel 400 or Hastelloy that the product, which receives the material of kettle,；
Preferably, the outer wall that the product receives kettle is provided with collet；
Preferably, the material of the product trapping device includes carbon steel and/or 304 stainless steels；
Preferably, the outer wall of the product trapping device is provided with collet；
Preferably, it is provided with plate washer in the product trapping device, product trapping device is divided into two Room by the plate washer；
Preferably, the product vacuum pump includes any one in water-ring vacuum pump, piston type vacuum pump or Roots vaccum pump
Kind.
4. purifying plant according to claim 1-3, which is characterized in that the purifier units evaporate before being additionally provided with
Divide trap and front-end volatiles vacuum pump, the front-end volatiles trap is used to trap the light component of the top of the distillation column output, described
Front-end volatiles vacuum pump is connect with the gas vent of front-end volatiles trap；
Preferably, the material of the front-end volatiles trap includes carbon steel and/or 304 stainless steels；
Preferably, the outer wall of the front-end volatiles trap is provided with collet；
Preferably, it is provided with plate washer in the front-end volatiles trap, front-end volatiles trap is divided into two Room by the plate washer；
Preferably, the gas outlet of the front-end volatiles trap is provided with filter screen；
Preferably, the front-end volatiles vacuum pump includes any in water-ring vacuum pump, piston type vacuum pump or Roots vaccum pump
A combination of one or more.
5. purifying plant according to claim 3, which is characterized in that the product trapping device includes sequentially connected product
Trap A, product trapping device B and product vacuum pump, the gas vent of the product trapping device A and the product trapping device B's
Gas access connection；
Preferably, the product vacuum pump includes any one in water-ring vacuum pump, piston type vacuum pump or Roots vaccum pump
Kind or two or more combinations.
6. purifying plant according to claim 3, which is characterized in that the raw material feed unit is additionally provided with fusing trapping
Device, the fusing trap are connect with the gas vent of the melting kettle and melting medial launder respectively；
Preferably, the material of the fusing trap includes carbon steel and/or 304 stainless steels；
Preferably, the outer wall of the fusing trap is provided with collet；
Preferably, plate washer is provided in the fusing trap, the plate washer is divided into two Room for trap is melted；
Preferably, the gas outlet of the fusing trap is provided with filter screen.
7. purifying plant according to claim 1-6, which is characterized in that the melting kettle, piping filter, meter
It is folder that amount pump, melting medial launder, superheater, rectifying column, refining kettle, condenser and product, which receive the connecting line between kettle,
Set of tubes；
Preferably, the material of the jacketed piping includes any one in 304 stainless steels, Monel 400 or Hastelloy.
8. a kind of method using the described in any item purifying plant purification Bravos of claim 1-7, which is characterized in that described
Method includes the following steps:
(1) Bravo raw material is melted, the Bravo after fusing is heated to bubble point；
(2) rectifying is heated to the Bravo of bubble point, carries out refinement treatment to rectifying tower bottom product, traps product, obtain hexachloro-benzene
Bravo no more than 10ppm.
9. according to the method described in claim 8, it is characterized in that, Bravo content is in step (1) the Bravo raw material
90-99.5wt.%, preferably 95-99wt.%；
Preferably, hexachlorobenzene content is 10-100ppm, preferably 30-80ppm in the Bravo raw material；
Preferably, the temperature of the fusing is 260-350 DEG C, preferably 300-330 DEG C；
Preferably, the bubble point temperature is 260-350 DEG C, preferably 300-330 DEG C；
Preferably, the stripping section temperature of step (2) described rectifying is 300-350 DEG C, preferably 320-330 DEG C；
Preferably, the rectifying section temperature of the rectifying is 260-330 DEG C, preferably 280-300 DEG C；
Preferably, the tower top absolute vacuum degree of the rectifying is 0.05-0.095MPa, preferably 0.06-0.08MPa；
Preferably, the overhead condenser temperature of the rectifying is 250-330 DEG C, preferably 260-290 DEG C；
Preferably, the tower bottom reboiler temperature of the rectifying is 300-350 DEG C, preferably 310-330 DEG C；
Preferably, the temperature of the refinement treatment is 260-350 DEG C, preferably 300-330 DEG C；
Preferably, the vacuum degree of the refinement treatment is 0.05-0.095MPa, preferably 0.06-0.08MPa；
Preferably, the temperature of the trapping is 40-150 DEG C, preferably 60-80 DEG C.
10. method according to claim 8 or claim 9, which is characterized in that described method includes following steps:
(1) 260-350 DEG C of fusing hexachlorobenzene content is 10-100ppm Bravo raw material, and is heated to 260-350 DEG C of bubble point temperature
It spends, Bravo content is 90-99.5wt.% in Bravo raw material；
(2) rectifying is heated to the Bravo of bubble point, and stripping section temperature is 300-350 DEG C, and rectifying section temperature is 260-330 DEG C, essence
The tower top absolute vacuum degree evaporated is 0.05-0.095MPa, and overhead condenser temperature is 250-330 DEG C, and tower bottom reboiler temperature is
300-350 DEG C, refinement treatment is carried out to tower bottom product, the temperature of refinement treatment is 260-350 DEG C, and the vacuum degree of refinement treatment is
0.05-0.095MPa, 40-150 DEG C trap the product after purification, obtain Bravo of the hexachloro-benzene no more than 10ppm and produce
Product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811486502.4A CN109293529B (en) | 2018-12-06 | 2018-12-06 | Purifying device and method for producing chlorothalonil with content of hexachlorobenzene not more than 10ppm |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811486502.4A CN109293529B (en) | 2018-12-06 | 2018-12-06 | Purifying device and method for producing chlorothalonil with content of hexachlorobenzene not more than 10ppm |
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| CN107056650A (en) * | 2016-10-20 | 2017-08-18 | 江苏维尤纳特精细化工有限公司 | The preparation of high-purity Bravo |
| CN207576343U (en) * | 2017-11-18 | 2018-07-06 | 江阴苏利化学股份有限公司 | A kind of low content Bravo refining plant |
| CN108329235A (en) * | 2018-03-02 | 2018-07-27 | 天津赛普泰克科技有限公司 | A kind of process producing high-purity Bravo |
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|---|---|---|---|---|
| JP2001213856A (en) * | 2000-01-28 | 2001-08-07 | Msk Management Kk | Method of purification for 2,4,5,6-tetrachloro-1,3- benzenedicarbonitrile |
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| CN104447407A (en) * | 2014-12-08 | 2015-03-25 | 江阴苏利化学股份有限公司 | Method of preparing chlorothalonil with hexachlorobenzene content lower than 10ppm |
| CN107056650A (en) * | 2016-10-20 | 2017-08-18 | 江苏维尤纳特精细化工有限公司 | The preparation of high-purity Bravo |
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