CN102180760B - Method for preparing benzene-free heptane solvent - Google Patents

Method for preparing benzene-free heptane solvent Download PDF

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Publication number
CN102180760B
CN102180760B CN 201110070163 CN201110070163A CN102180760B CN 102180760 B CN102180760 B CN 102180760B CN 201110070163 CN201110070163 CN 201110070163 CN 201110070163 A CN201110070163 A CN 201110070163A CN 102180760 B CN102180760 B CN 102180760B
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heptane
tower
benzene
removing column
solvent
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CN102180760A (en
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张殿明
李荣忠
谢海鹰
朱彦斌
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Beijing Yanshan Jilian Petroleum Chemical Co., Ltd.
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BEIJING YANSHAN JILIAN PETROLEUM CHEMICAL Co Ltd
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Abstract

The invention discloses a method for preparing a benzene-free heptane solvent, which comprises the following steps of: (1) removing light components, namely adding cutting oil from which hexane is extracted into a light-removing tower, and removing the light components on the tower top, wherein effluent at the tower bottom is crude heptane from which the light components are removed; (2) removing heavy components, namely adding the crude heptane from which the light components are removed in the step (1) into a heavy-removing tower, and collecting the crude heptane from which the heavy components are removed on the tower top, wherein effluent at the tower bottom is mixed liquid containing intermediate and heavy components; and (3) performing catalytic hydrogenation, namely performing catalytic hydrogenation reaction on the crude heptane from which the heavy components are removed in the step (2) by using a hydrogenation reactor to convert aromatic hydrocarbon into alkane, and introducing gas obtained after reaction liquid is separated by a separation tank into a condenser for condensing, wherein the condensed liquid is the benzene-free heptane solvent. The process is simple and suitable for industrial production, the yield of the heptane is over 80 percent, and the blank of (environment-friendly) mass industrial production of the benzene-free heptane solvent in China is filled; and good economic benefits and social benefits are achieved.

Description

A kind of method for preparing no benzene heptane solvent
Technical field
The present invention relates to a kind of method for preparing no benzene heptane solvent, belong to chemical production field.
Background technology
Series (environmental protection) normal heptane solvent is a very wide industrial solvent of a kind of application.At present, China can only produced in small quantities contain the aromatic hydrocarbons heptane solvent, along with petrochemical complex, medicine, the continuous development of foodstuffs industry, some performance of this technical grade solvent can not be satisfied the demand, and exploitation series (content difference) environment-friendly and green does not have the benzene normal heptane solvent, increases range of product, improve product hierarchy and be our instant task of enterprise, this also is to improve the enterprise competitiveness effective way under the market economy.
Summary of the invention
The technical problem to be solved in the present invention is to overcome existing defective, but provides the simple industrial scale production of a kind of technology, environmental protection not to have the method for not having the benzene heptane solvent fully of benzene.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
A kind of method for preparing no benzene heptane solvent is a raw material with the cutting oil after the hexane extracting, comprises the steps:
(1) remove light constituent: the cutting oil after the hexane extracting enters lightness-removing column, make the still temperature maintain 104 ± 2 ℃, tower top temperature is controlled at 98 ± 2 ℃, slough light constituent from cat head, light constituent part after condenser condenses is delivered to storage tank, a part is delivered to trim the top of column, and tower still effluent liquid is the thick heptane that removes behind the light constituent;
(2) remove heavy constituent: the thick heptane after step (1) removes heavy constituent enters weight-removing column, 132 ± 2 ℃ of control tower still temperature, 120 ± 2 ℃ of tower top temperatures, collect the thick heptane that removes heavy constituent from cat head, a part is delivered to the weight-removing column cat head as backflow after condenser condenses, and tower still liquid effluent is the mixed solution of heavy constituent in containing;
(3) shortening: the thick heptane that removes in the step (2) after the heavy constituent is changed into alkane through hydrogenator generation catalytic hydrogenation reaction with aromatic hydrocarbons, the gas of reaction solution after separating tank separates enters condenser and carries out condensation, and condensed liquid is no benzene heptane solvent.
Catalytic hydrogenation reaction adopts the NCG catalyst as catalyzer in the step (3).
Further, regulate the temperature of the tower still of lightness-removing column in step (1), the step (2) respectively by tower still reboiler.
Further, the cutting oil after the raw material hexane extracting in the step (1) is delivered to the dehydrogenation tower again after with the preheating of lightness-removing column tower still effluent liquid and is removed light constituent.
Further, the reorganization dispensing hexane production plant that removes by weight-removing column in the step (2) is as the raw material of producing hexane.
Beneficial effect of the present invention is as follows:
Cutting oil after hexane extracting normal heptane content in the material that the primary tower pre-treatment obtains removes light constituent in the component simultaneously more than 25%; Further this material is handled through rectifying tower, it more than 40% is heptane that cat head obtains again; This material is through rectifying separation, obtains massfraction and be 40%-90% normal heptane, heavy constituent mixed solution during the tower still flows out and contains; After hydrogenator changes into alkane with aromatic hydrocarbons, obtain the no benzene heptane solvent finished product of massfraction 40-90% series, technology of the present invention is simple, but suitability for industrialized production, the heptane yield reaches more than 80%, fills up the blank that the production of domestic (environmental protection) industrial scale does not have the benzene heptane solvent; Produce favorable economic benefit and social benefit.
Description of drawings
Accompanying drawing is used to provide further understanding of the present invention, and constitutes the part of specification sheets, is used from explanation the present invention with embodiments of the invention one, is not construed as limiting the invention.In the accompanying drawings:
Fig. 1, Fig. 2 are the process flow sheets that the present invention prepares the method for no benzene heptane solvent.
Embodiment
Below in conjunction with accompanying drawing the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein only is used for description and interpretation the present invention, and be not used in qualification the present invention.
Embodiment 1
Be raw material with the cutting oil after the hexane extracting when method that the preparation described in the present invention does not have a benzene heptane solvent is produced heptane, adopt two tower rectifying, one tower removes light constituent, two towers remove heavy constituent, obtain 80% thick heptane product (toluene that contains massfraction about 1%), carry out under catalysis, adopting liquid-phase hydrogenatin to remove toluene to containing the thick heptane of toluene about 1% then, obtain the 80%(massfraction) smart heptane product.
Concrete technical process is as follows: as Fig. 1, shown in Figure 2, label A among Fig. 1, B, C, the lines of D respectively with Fig. 2 in label A, B, C, the lines of D ' connect one to one, cutting oil after the hexane extracting is from head tank 11,12 after the tower bottoms preheating that interchanger 3 usefulness lightness-removing columns 4 tower bottom flows go out, by fresh feed pump 801,802 pump into lightness-removing column 4 removes lower boiling light constituent, the lower boiling light constituent that cat head distills out enters condenser 61,62 carry out condensation, uncooled tail gas high altitude discharge, condensed light constituent enters in the return tank 7, part light constituent is pumped in the storage tank 9 through pump 806, part light constituent is sent lightness-removing column 4 trim the top of column back to by reflux pump 805,104 ± 2 ℃ of lightness-removing column 4 tower still temperature controls, tower top temperature is controlled at 98 ± 2 ℃, regulate tower still temperature by the tower bottom reboiler 5 that is arranged at the bottom of lightness-removing column 4 towers, tower bottoms pump 803,804 are pumped in the weight-removing column 14 and remove heavy constituent, 132 ± 2 ℃ of weight-removing column 14 still temperature controls, 120 ± 2 ℃ of tower top temperatures, regulate the still temperature by the tower bottom reboiler 13 that is arranged at the bottom of the tower, cat head steams thing through condenser 15,16 are cooled to 40 ℃ and 20 ℃, flow into respectively in the return tank 24, the thick heptane of a part uses pump 812 to send weight-removing column 14 trim the top of column back to, the thick heptane product of a part is pumped to thick heptane jar 251 with pump 813,252, in 253, still liquid is after tower still interchanger 10 is cooled to 50 ℃, a part is pumped into tower bottom reboiler 5 through pump 807 and is used to regulate temperature in the tower, another part is sent in the bottom product jar 18 through pump 808, through pump 810,811 are delivered to the hexane production plant as the sherwood oil product.
After lightness-removing column 4 and 14 liang of tower rectifying of weight-removing column, be stored in the thick heptane (aromatic hydrocarbons that contains massfraction 1.2% in the thick heptane) in the thick heptane jar 251,252,253, to be pumped in the preheater 17 with fresh feed pump 809, be preheating to 140 ~ 150 degree, hydrogen is entered in the mixing tank 26 behind the thorough mixing with thick heptane behind the 11.2NM3 through Flow-rate adjustment through the 0.8 ~ 0.9Mpa that reduces pressure by hexane workshop 2.8 ~ 3Mpa again, enter in the hydrogenator 19, under the effect of CNG catalyst, change into alkane behind the aromatic hydrogenation in the thick heptane.After reaction solution enters and separates in the vapor-liquid separation tank 20, during liquid enters after the water cooler cooling and stores up in the storage tank, gas is behind the tank deck condenser, enter water cooler, the liquid solvent oil that condensation is got off is content 80%(massfraction) smart heptane, deliver in the smart heptane product jar, noncondensable gas enters the torch house steward.
It should be noted that at last: the above only is the preferred embodiments of the present invention, be not limited to the present invention, although the present invention is had been described in detail with reference to previous embodiment, for a person skilled in the art, it still can be made amendment to the technical scheme that aforementioned each embodiment put down in writing, and perhaps part technical characterictic wherein is equal to replacement.Within the spirit and principles in the present invention all, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (5)

1. a method for preparing no benzene heptane solvent is characterized in that, is raw material with the cutting oil after the hexane extracting, comprises the steps:
(1) remove light constituent: the cutting oil after the hexane extracting enters lightness-removing column, make the still temperature maintain 104 ± 2 ℃, tower top temperature is controlled at 98 ± 2 ℃, slough light constituent from cat head, light constituent part after condenser condenses is delivered to storage tank, a part is delivered to trim the top of column, and tower still effluent liquid is the thick heptane that removes behind the light constituent;
(2) remove heavy constituent: the thick heptane after step (1) removes light constituent enters weight-removing column, 132 ± 2 ℃ of control tower still temperature, 120 ± 2 ℃ of tower top temperatures, collect the thick heptane that removes heavy constituent from cat head, a part is delivered to the weight-removing column cat head as backflow after condenser condenses, and tower still liquid effluent is the mixed solution of heavy constituent in containing;
(3) shortening: the thick heptane that removes in the step (2) after the heavy constituent is transformed alkane through hydrogenator generation catalytic hydrogenation reaction with aromatic hydrocarbons, the gas of reaction solution after separating tank separates enters condenser and carries out condensation, and condensed liquid is no benzene heptane solvent.
2. preparation according to claim 1 does not have the method for benzene heptane solvent, it is characterized in that, catalytic hydrogenation reaction adopts the NCG catalyst as catalyzer in the step (3).
3. preparation according to claim 1 does not have the method for benzene heptane solvent, it is characterized in that, regulates the temperature of the tower still of lightness-removing column or weight-removing column in step (1), the step (2) respectively by tower still reboiler.
4. preparation according to claim 1 does not have the method for benzene heptane solvent, it is characterized in that, the cutting oil after the raw material hexane extracting in the step (1) is delivered to lightness-removing column again after with the preheating of lightness-removing column tower still effluent liquid and removed light constituent.
5. preparation according to claim 1 does not have the method for benzene heptane solvent, it is characterized in that, the reorganization dispensing hexane production plant that removes by weight-removing column in the step (2) is as the raw material of producing hexane.
CN 201110070163 2011-03-23 2011-03-23 Method for preparing benzene-free heptane solvent Active CN102180760B (en)

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CN107586249A (en) * 2016-07-08 2018-01-16 中国石化扬子石油化工有限公司 A kind of method of the adsorbing and removing aromatic hydrocarbons from alkane solvent
RU2714310C1 (en) * 2019-05-06 2020-02-14 Общество с ограниченной ответственностью "Газпром трансгаз Екатеринбург" Solvent based on heavy hydrocarbons
CN110003007A (en) * 2019-05-10 2019-07-12 安阳永金化工有限公司 Coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system and method
CN111072441A (en) * 2019-12-29 2020-04-28 宁夏百川通清洁能源有限公司 Method for removing aromatic hydrocarbon from n-heptane

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN1872820A (en) * 2006-04-03 2006-12-06 南京师范大学 Method for distilling normal heptane and methyl - cyclohexane by using combination of rectification and compound extracted rectification

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN1872820A (en) * 2006-04-03 2006-12-06 南京师范大学 Method for distilling normal heptane and methyl - cyclohexane by using combination of rectification and compound extracted rectification

Non-Patent Citations (4)

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Title
从直馏汽油分级分离正庚烷及甲基环己烷;刘晶等;《常州大学学报(自然科学版)》;20100930;第22卷(第3期);34-37 *
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