CN1208727A - Continuous distillation technology for coking naphthalene oil fraction - Google Patents

Continuous distillation technology for coking naphthalene oil fraction Download PDF

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Publication number
CN1208727A
CN1208727A CN97107637A CN97107637A CN1208727A CN 1208727 A CN1208727 A CN 1208727A CN 97107637 A CN97107637 A CN 97107637A CN 97107637 A CN97107637 A CN 97107637A CN 1208727 A CN1208727 A CN 1208727A
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Prior art keywords
naphthalene
fraction
acenaphthene
oil
methylnaphthalene
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CN97107637A
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何雪峰
李应海
童晓宇
张初永
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Coal Chemical Co Panzhihua Iro
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Coal Chemical Co Panzhihua Iro
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Priority to CN97107637A priority Critical patent/CN1208727A/en
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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Abstract

The invention discloses a new technology for deep processing of coal coking byproduct washing oil, namely, a three-furnace three-tower hot oil continuous rectification processing technology is adopted, various chemical products such as industrial naphthalene, industrial methylnaphthalene, industrial acenaphthene fraction, dibenzofuran fraction and the like can be simultaneously processed, and the technology has the advantages of energy conservation, investment saving and high production efficiency, and provides a new way for processing the coal coking byproduct.

Description

Coking naphtalene oil fraction continuous rectification technology
The invention belongs to coal tar by-product oil naphthalene and washing oil deep process technology field, especially relate to naphtalene oil and washing oil deep fat and connect material " three stoves, three towers " rectification process technology.
The coal tar industry has also been brought multiple coal tar byproduct, as naphtalene oil and washing oil except that production metallurgy Jiao.Deep processing (rectifying separation) to these byproducts has economic worth and practical value widely.
In the deep processing prior art to naphtalene oil and washing oil, general " twin furnace double tower " technology that adopts is promptly utilized each fore-running tube furnace, rectifying tube furnace, primary tower and a rectifying tower, to wash the complete processing that blending fraction carries out as raw material.
To NAPTHALENE FLAKES. (INDUSTRIAL GRADE, technical methylnaphthalene production, to wash the blending fraction raw material and carry out fore-running at primary tower, deviate from the carbolic oil fraction at the primary tower top, extract out by hot oil pump at primary tower bottom Residual oil and send fore-running tubular oven round-robin simultaneously, extract wherein a part of raw material out as rectifying tower.Rectifying tower top obtains NAPTHALENE FLAKES. (INDUSTRIAL GRADE, and the Residual oil of rectifier bottoms outputs to the hydronic while of rectifying tubular oven, and the extraction unit dispensing causes water cooler and is cooled to 90~110 ℃, then becomes the washing oil product.If want further processing industry methylnaphthalene, to be raw material (about 60 ℃) then with the above-mentioned washing oil that obtains, send into rectifying tower and carry out technical methylnaphthalene " single tower " flow process, then this moment, rectifying tower top was deviate from technical methylnaphthalene, and the bottom obtains remaining naphtalene oil.This technology exists obviously not enough:
(1) simultaneously manufacture naphthalene, technical methylnaphthalene.If will produce two kinds of goods, then need two to overlap independently distillation system, invest too big;
(2) because technical methylnaphthalene is to reheat back (from 60 ℃ → 280 ℃) from the washing oil that takes off NAPTHALENE FLAKES. (INDUSTRIAL GRADE to enter rectifying tower and separate, causes and repeat power consumption, increased production cost.
For " twin furnace double tower " complete processing of acenaphthene fraction, dibenzofuran fraction, be similar to " twin furnace double tower " complete processing of NAPTHALENE FLAKES. (INDUSTRIAL GRADE and technical methylnaphthalene, be raw material just with demethylation naphthalene washing oil, also there is similar problem:
(1) acenaphthene fraction, dibenzofuran fraction can not synchronous production;
(2) need reheat owing to taking off the acenaphthene Residual oil, cause and repeat power consumption, increase production cost.
The objective of the invention is, adopt coking naphtalene oil fraction deep fat to connect material " three stoves, three towers " distillation technology, and make NAPTHALENE FLAKES. (INDUSTRIAL GRADE and technical methylnaphthalene or acenaphthene fraction and dibenzofuran fraction synchronous production, simultaneously, reduce the heating that repeats of taking off the NAPTHALENE FLAKES. (INDUSTRIAL GRADE Residual oil and taking off acenaphthene fraction Residual oil, play the effect of energy efficiency.
Coking naphtalene oil fraction continuous rectification technology is to be raw material with coal tar byproduct washing oil, processes continuously through " three stoves, three towers " equipment, makes the technology of NAPTHALENE FLAKES. (INDUSTRIAL GRADE and technical methylnaphthalene or acenaphthene fraction and dibenzofuran fraction, it is characterized in that:
(1) on the basis of " twin furnace double tower " equipment of general usefulness, set up one on one of identical rectifying tubular oven of class Sihe and rectifying tower, promptly form " three stoves, three towers " processing units;
(2) deep fat that takes off the naphthalene Residual oil or take off the acenaphthene Residual oil from the output of preposition rectifying tower directly enters rearmounted rectifying tower processing, makes technical methylnaphthalene and dibenzofuran fraction respectively from rearmounted rectifying tower top;
(3) the output of rearmounted rectifier bottoms take off technical methylnaphthalene or deoxidation fluorenes fraction Residual oil enters rearmounted rectifying tubular oven round-robin simultaneously, extract the part Residual oil out and cool off, make and take off the naphthalene washing oil or take off the acenaphthene washing oil.
Further, aforesaid coking naphtalene oil fraction continuous rectification technology, the coking naphtalene oil fractional composition of being adopted for (weight, %): other unknown material of indenes naphthalene beta-methylnaphthalene alpha-methyl-naphthalene biphenyl 0.8-1.0 40.0-50.0 10.0-13.0 5.0-7.0 3.0-4.0 dimethylnaphthalene acenaphthene dibenzofuran fluorenes 9.0-11.0 8.0-10.0 4.5-5.5 5.5-6.5 3.5-4.5
Further, aforesaid coking naphtalene oil fraction continuous rectification technology, its controlled variable is:
260~300 ℃ of 170~260 ℃ of fore-running column bottom temperatures of fore-running tower top temperature
280~315 ℃ of 220~280 ℃ of preposition rectifying column bottom temperatures of preposition rectifying tower top temperature
280~320 ℃ of 235~295 ℃ of rearmounted rectifying column bottom temperatures of rearmounted rectifying tower top temperature
Reflux ratio is not less than 2 treatment capacities, 3.5~4.2T/h
Further, aforesaid coking naphtalene oil fraction continuous rectification technology, the chemical constitution of prepared NAPTHALENE FLAKES. (INDUSTRIAL GRADE be (weight, %):
Other unknown material of indenes naphthalene dimethylnaphthalene acenaphthene
0.05-0.20 98.0-99.8 0.005-0.01 0.05-0.10 0.001-0.010
The chemical constitution of prepared technical methylnaphthalene be (weight, %):
Naphthalene beta-methylnaphthalene alpha-methyl-naphthalene biphenyl
2.5-3.5 45.8-55.0 23.5-25.5 13.6-15.5
Two basic other unknown materials of first naphthalene
4.0-5.0 0.40-0.55
The chemical constitution of prepared acenaphthene fraction be (weight, %):
Indenes naphthalene beta-methylnaphthalene biphenyl dimethylnaphthalene
0.020-0.03 0.01-0.03 0.05-0.10 0.2-0.40 22.5-25.0
Other unknown material of acenaphthene dibenzofuran
58.0-65.0 10.7-12.7 0.32-0.52
The chemical constitution of prepared dibenzofuran fraction be (weight, %):
Indenes naphthalene beta-methylnaphthalene alpha-methyl-naphthalene biphenyl
0.04-0.10 0.05-0.20 0.10-0.37 0.08-0.24 0.10-0.30
Other unknown material of dimethylnaphthalene acenaphthene dibenzofuran fluorenes
2.00-3.50 14.0-15.5 50.0-60.0 16.8-18.6 5.0-6.0
According to polycomponent rectifying principle, use common rectifying tower, when separating four component solutions in the continuous rectification mode, then need three towers, that is to say coking by-products naphtalene oil fraction is produced carbolic oil, NAPTHALENE FLAKES. (INDUSTRIAL GRADE, technical methylnaphthalene and four kinds of products of demethylation naphthalene washing oil simultaneously, perhaps separating lightweight washing oil, acenaphthene, dibenzofuran and four kinds of products of fluorenes in the demethylation naphthalene washing oil simultaneously, is feasible in theory.
Adopt coking naphtalene oil fraction continuous rectification technology of the present invention, have following advantage:
(1) can the synchronous production multiple product, as carbolic oil, NAPTHALENE FLAKES. (INDUSTRIAL GRADE, technical methylnaphthalene and demethylation naphthalene; Perhaps the lightweight washing oil in the demethylation naphthalene washing oil, acenaphthene, dibenzofuran and fluorenes goods;
(2) owing to reduced the loss of intermediates, increased the output of rectifying goods;
(3) owing to intermediates need not then can save the energy greatly through cooling reheat process.
Accompanying drawing is coking naphtalene oil fraction of the present invention continuous rectification " three stoves, three a towers " process flow sheet.
201,202,203 be respectively primary tower, preposition rectifying tower and rearmounted rectifying tower, its top discharge port is respectively 2,3,4, its bottom discharge mouth is respectively 12,13,14, and feeding mouth is respectively 5,6,7 in the middle of it, and the feeding mouth that is connected with process furnace is respectively 9,10,11;
101,102,103 be respectively fore-running tubular oven, preposition rectifying tubular oven and rearmounted rectifying tubular oven, it is respectively 15,16,17 with primary tower 201, preposition rectifying tower 202 and the discharge port that rearmounted rectifying tower 203 is connected, and its opening for feed is respectively 18,19,20.
Below in conjunction with drawings and Examples design of the present invention is further elaborated.
Embodiment 1
Realization separates the continuous rectification technology of carbolic oil, NAPTHALENE FLAKES. (INDUSTRIAL GRADE, technical methylnaphthalene and demethylation naphthalene washing oil from coking naphtalene oil fraction.
With temperature is that 205 ℃ naphtalene oil fraction 1 is sent into primary tower 201 from primary tower opening for feed 5 with the inlet amount of 3.5~4.0t/h, top discharge port 2 from primary tower 201 after fore-running is isolated carbolic oil, the tower bottoms of primary tower 201 partly enters fore-running tubular oven 101 heating cycle, part is directly sent into preposition rectifying tower 202, after rectifying, isolate NAPTHALENE FLAKES. (INDUSTRIAL GRADE from preposition rectifying tower 202 top discharge ports 3, preposition rectifying tower 202 bottom Residual oils partly enter preposition rectifying tubular oven 102 heating cycle, part directly enters rearmounted rectifying tower 203 and carries out rectifying, isolate technical methylnaphthalene from rearmounted rectifying tower 203 top discharge mouths 4, and the bottom Residual oil of rearmounted rectifying tower 203 partly enters rearmounted rectifying tubular oven 103 heating cycle; Demethylation naphthalene washing oil product is isolated from discharge port 14 in part cooling back.
Aforesaid technology, its controlled variable is:
260~280 ℃ of primary tower 201 top temperature 170~185 ℃ of 201 ends of primary tower temperature
280~290 ℃ of rectifying tower 202 top temperature 220~230 ℃ of 202 ends of rectifying tower temperature
280~300 ℃ of rectifying tower 203 top temperature 235~245 ℃ of 203 ends of rectifying tower temperature
Reflux ratio is not less than 3 treatment capacities, 3.5~4T/h
The chemical constitution of prepared goods be (weight, %):
NAPTHALENE FLAKES. (INDUSTRIAL GRADE
Other unknown material of indenes naphthalene dimethylnaphthalene acenaphthene
0.05-0.20 98.0-99.8 0.005-0.01 0.05-0.10 0.001-0.010
Technical methylnaphthalene
Naphthalene beta-methylnaphthalene alpha-methyl-naphthalene biphenyl
2.5-3.5 45.8-55.0 23.5-25.5 13.6-15.5
Two basic other unknown materials of first naphthalene
4.0-5.0 0.40-0.55
Embodiment 2
From demethylation naphthalene washing oil, isolate the continuous rectification technology of lightweight washing oil, acenaphthene, dibenzofuran and four kinds of products of fluorenes.
Its procedure of processing is similar to Example 1.
Demethylation naphthalene washing oil raw material enters primary tower 201 from opening for feed 5, isolates lightweight washing oil, acenaphthene fraction and dibenzofuran fraction from the top of primary tower 201, preposition rectifying tower 202 and rearmounted rectifying tower 203 respectively, isolates fluorenes fraction 8 from rearmounted rectifier bottoms.
Aforesaid technology, its controlled variable is:
290~300 ℃ of primary tower 201 top temperature 250~260 ℃ of 201 ends of primary tower temperature
295~315 ℃ of rectifying tower 202 top temperature 270~280 ℃ of 202 ends of rectifying tower temperature
310~320 ℃ of rectifying tower 203 top temperature 285~295 ℃ of 203 ends of rectifying tower temperature
Reflux ratio is not less than 2 treatment capacities, 4~4.2T/h
The chemical constitution of prepared goods be (weight, %):
The acenaphthene fraction:
Indenes naphthalene beta-methylnaphthalene biphenyl dimethylnaphthalene
0.020-0.03 0.01-0.03 0.05-0.10 0.2-0.40 22.5-25.0
Other unknown material of acenaphthene dibenzofuran
58.0-65.0 10.7-12.7 0.32-0.52
The dibenzofuran fraction:
Indenes naphthalene beta-methylnaphthalene alpha-methyl-naphthalene biphenyl
0.04-0.10 0.05-0.20 0.10-0.37 0.08-0.24 0.10-0.30
Other unknown material of dimethylnaphthalene acenaphthene dibenzofuran fluorenes
2.00-3.50 14.0-15.5 50.0-60.0 16.8-18.6 5.0-6.0。

Claims (4)

1. coking naphtalene oil fraction continuous rectification technology is to be raw material with coal tar byproduct mixing naphtalene oil, processes continuously through " three stoves, three towers " equipment, makes the technology of NAPTHALENE FLAKES. (INDUSTRIAL GRADE and technical methylnaphthalene or acenaphthene fraction and dibenzofuran fraction, it is characterized in that:
(1) on the basis of general " twin furnace double tower " equipment, set up one on one of similar or identical rectifying tubular oven and rectifying tower, promptly form " three stoves, three towers " processing units;
(2) deep fat that takes off the naphthalene Residual oil or take off the acenaphthene Residual oil from the output of preposition rectifier bottoms directly enters rearmounted rectifying tower processing, makes technical methylnaphthalene and dibenzofuran fraction respectively from rearmounted rectifying tower top;
(3) Residual oil that takes off technical methylnaphthalene or deoxidation fluorenes fraction in rearmounted rectifier bottoms output enters rearmounted rectifying tubular oven round-robin simultaneously, extracts the part Residual oil out and cools off, and makes and takes off the naphthalene washing oil or take off the acenaphthene washing oil.
2. coking naphtalene oil fraction continuous rectification technology as claimed in claim 1, it is characterized in that, the fractional composition of described coking naphtalene oil be (weight, %): other unknown material of indenes naphthalene beta-methylnaphthalene alpha-methyl-naphthalene biphenyl 0.8-1.0 40.0-50.0 10.0-13.0 5.0-7.0 3.0-4.0 dimethylnaphthalene acenaphthene dibenzofuran fluorenes 9.0-11.0 8.0-10.0 4.5-5.5 5.5-6.5 3.5-4.5
3. as claim 1,2 described coking naphtalene oil fraction continuous rectification technology is characterized in that:
260~300 ℃ of 170~260 ℃ of fore-running column bottom temperatures of fore-running tower top temperature
280~315 ℃ of 220~280 ℃ of preposition rectifying column bottom temperatures of preposition rectifying tower top temperature
280~320 ℃ of 235~295 ℃ of rearmounted rectifying column bottom temperatures of rearmounted rectifying tower top temperature
Reflux ratio is not less than 2 treatment capacities, 3.5~4.2T/h
4. as the described coking naphtalene oil of claim 1,2 or 3 fraction continuous rectification technology, it is characterized in that,
The chemical constitution of described goods NAPTHALENE FLAKES. (INDUSTRIAL GRADE be (weight, %):
Other unknown material of indenes naphthalene dimethylnaphthalene acenaphthene
0.05-0.20 98.0-99.8 0.005-0.01 0.05-0.10 0.001-0.010
The chemical constitution of described goods technical methylnaphthalene be (weight, %):
Naphthalene beta-methylnaphthalene alpha-methyl-naphthalene biphenyl
2.5-3.5 45.8-55.0 23.5-25.5 13.6-15.5
Two basic other unknown materials of first naphthalene
4.0-5.0 0.40-0.55
The chemical constitution of described goods acenaphthene fraction be (weight, %):
Indenes naphthalene beta-methylnaphthalene biphenyl dimethylnaphthalene
0.020-0.03 0.01-0.03 0.05-0.10 0.2-0.40 22.5-25.0
Other unknown material of acenaphthene dibenzofuran
58.0-65.0 10.7-12.7 0.32-0.52
The chemical constitution of described goods dibenzofuran fraction be (weight, %):
Indenes naphthalene beta-methylnaphthalene alpha-methyl-naphthalene biphenyl
0.04-0.10 0.05-0.20 0.10-0.37 0.08-0.24 0.10-0.30
Other unknown material of dimethylnaphthalene acenaphthene dibenzofuran fluorenes
2.00-3.50 14.0-15.5 50.0-60.0 16.8-18.6 5.0-6.0
CN97107637A 1997-08-14 1997-08-14 Continuous distillation technology for coking naphthalene oil fraction Pending CN1208727A (en)

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Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
CN97107637A CN1208727A (en) 1997-08-14 1997-08-14 Continuous distillation technology for coking naphthalene oil fraction

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CN1208727A true CN1208727A (en) 1999-02-24

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100336788C (en) * 2004-12-07 2007-09-12 哈尔滨工程大学 Method of extracting high purity acenaphthene from coat tar scrubbing oil
CN101302447A (en) * 2008-05-14 2008-11-12 莱芜市泰山焦化有限公司 Method for changing benzol scrubber to scrub oil when resistance rises in winter
CN101899313A (en) * 2010-07-29 2010-12-01 河南宝硕焦油化工有限公司 Oil-washing deep processing technology of coal tar
CN101982523A (en) * 2010-11-24 2011-03-02 孝义市金精化工有限公司 Washing oil continuous processing method
CN102731282A (en) * 2012-07-12 2012-10-17 韩钊武 Method for extracting dibenzofuran from absorber oil of coal tar
CN101643380B (en) * 2008-08-08 2013-04-10 鞍钢集团工程技术有限公司 Process for producing industrial fluorene by coal tar wash oil
CN107129422A (en) * 2016-02-28 2017-09-05 华东理工大学 The continuous distillation method of high-purity biphenyl is extracted in a kind of tower first raffinate from crude benzol
CN112933633A (en) * 2021-04-12 2021-06-11 孝义市金精化工有限公司 Negative-pressure continuous distillation and separation device for coal tar washing oil and coal tar washing oil separation and refining method

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100336788C (en) * 2004-12-07 2007-09-12 哈尔滨工程大学 Method of extracting high purity acenaphthene from coat tar scrubbing oil
CN101302447A (en) * 2008-05-14 2008-11-12 莱芜市泰山焦化有限公司 Method for changing benzol scrubber to scrub oil when resistance rises in winter
CN101302447B (en) * 2008-05-14 2013-04-10 莱芜市泰山焦化有限公司 Method for exchanging changing absorber oil in benzol scrubber when resistance rises in winter
CN101643380B (en) * 2008-08-08 2013-04-10 鞍钢集团工程技术有限公司 Process for producing industrial fluorene by coal tar wash oil
CN101899313A (en) * 2010-07-29 2010-12-01 河南宝硕焦油化工有限公司 Oil-washing deep processing technology of coal tar
CN101982523A (en) * 2010-11-24 2011-03-02 孝义市金精化工有限公司 Washing oil continuous processing method
CN101982523B (en) * 2010-11-24 2013-03-20 孝义市金精化工有限公司 Washing oil continuous processing method
CN102731282A (en) * 2012-07-12 2012-10-17 韩钊武 Method for extracting dibenzofuran from absorber oil of coal tar
CN107129422A (en) * 2016-02-28 2017-09-05 华东理工大学 The continuous distillation method of high-purity biphenyl is extracted in a kind of tower first raffinate from crude benzol
CN112933633A (en) * 2021-04-12 2021-06-11 孝义市金精化工有限公司 Negative-pressure continuous distillation and separation device for coal tar washing oil and coal tar washing oil separation and refining method

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