CN113004112A - Isohexane preparation process - Google Patents

Isohexane preparation process Download PDF

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Publication number
CN113004112A
CN113004112A CN202110241167.7A CN202110241167A CN113004112A CN 113004112 A CN113004112 A CN 113004112A CN 202110241167 A CN202110241167 A CN 202110241167A CN 113004112 A CN113004112 A CN 113004112A
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acid
tank
reaction
alkali
solution
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达力
蒋超
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CHUZHOU RUNDA SOLVENTS CO LTD
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CHUZHOU RUNDA SOLVENTS CO LTD
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/005Processes comprising at least two steps in series
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/04Purification; Separation; Use of additives by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/10Purification; Separation; Use of additives by extraction, i.e. purification or separation of liquid hydrocarbons with the aid of liquids

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses an isohexane preparation process, which comprises the following steps: carrying out vapor-liquid separation on raw materials, preparing distillate, and preparing acid-washed materials and finished products; the method comprises the steps of heating and reacting raw oil to a rectification reaction state of gas-liquid separation through a rectification tower, preparing distillate and naphtha through condensation reflux, and then carrying out acid washing and alkali washing on the distillate in sequence to finally prepare the high-purity industrial isohexane.

Description

Isohexane preparation process
Technical Field
The invention relates to the technical field of isohexane production and preparation, and in particular relates to an isohexane preparation process.
Background
Isohexane is an organic compound, is colorless liquid, can be mixed and dissolved with acetone, benzene, chloroform, heptane, is soluble in ethanol and ether, is insoluble in water, has irritation, is mainly used for solvents for polymerization, cleaning and oil releasing agents of precise instruments and meters, essential oil diluents and the like, is mainly used in the product fields of nontoxic sprays, solvents, cleaning agents and the like, currently, isohexane is produced in partial oil refineries at home, the annual output is more than ten thousand tons, the isohexane is sold to all over the country on the basis of meeting the consumption of the factory, the sales condition is good, and the price is always in the rising trend in recent years due to the low isohexane output and large market demand;
at present, industrial isohexane prepared by autonomous production in China is still in a state of short supply and short demand, and most of isohexane used in industrial production depends on import, which is mainly caused by the fact that the existing isohexane preparation processes have overlong production lines and complicated equipment and operation, so that the preparation cost is high, the production efficiency is low, the processes are not suitable for large-scale production, in addition, the ecological environment is greatly polluted, and good economic benefits cannot be brought, so that the invention provides the isohexane preparation process to solve the problems in the prior art.
Disclosure of Invention
In order to solve the problems, the invention aims to provide an isohexane preparation process, which comprises the steps of heating and reacting raw oil to a rectification reaction state of vapor-liquid separation through a rectification tower, preparing distillate and naphtha through condensation reflux, and then carrying out acid washing and alkali washing on the distillate in sequence to finally prepare high-purity industrial isohexane.
In order to achieve the purpose of the invention, the invention is realized by the following technical scheme: a process for preparing isohexane comprises the following steps:
the method comprises the following steps: raw material vapor-liquid separation
Raw oil is pumped into a reactor at the bottom of a rectifying tower through a raw material pump, the raw oil is heated to react, and after the raw oil is heated for a specified time, materials in the reactor form a vapor-liquid state and enter a rectifying reaction state;
step two: distillate preparation
According to the first step, firstly, condensing steam in the materials in the rectifying tower through a condenser and refluxing the steam to a reflux tank to enable the steam-liquid two phases in the materials to be in countercurrent contact and realize interphase mass transfer to obtain high-purity volatile tower top distillate and high-purity nonvolatile tower bottom sediment, then guiding the distillate into a semi-finished product tank for temporary storage and standby application, and guiding the tower bottom sediment into a storage tank for storage to obtain naphtha for sale;
step three: acid pickling materials
According to the second step, firstly, putting acid solution with specified weight part into an enamel acid tank, then guiding distillate in a semi-finished product tank into the enamel acid tank and carrying out acid washing reaction with the acid solution, removing alkaline impurities and phenolic substances in the distillate, guiding mixed solution into a settling tank after the acid washing reaction is finished, and separating the materials from the acid solution to obtain the acid-washed materials;
step four: preparation of finished product
According to the third step, firstly, putting alkali solution with specified weight part into an enamel alkali tank, then introducing the material after acid washing into the enamel alkali tank and carrying out alkali washing reaction with the alkali solution, removing acid impurities in the material, introducing the reaction solution into a separation tank after the alkali washing reaction is finished, separating the material from the alkali solution to obtain the material after alkali washing, and then introducing the material after alkali washing into a finished product storage tank to obtain high-purity process isohexane.
The further improvement lies in that: in the first step, the raw oil heating source adopts high-temperature vacuum gas generated by a coal-fired steam boiler, the heating temperature in the reactor is controlled to be 80-90 ℃, and the heating reaction time is longer than 5 hours.
The further improvement lies in that: in the second step, the condensation reaction times are selected according to the purity of the materials required by production in the condensation process, volatile components in the liquid phase enter the gas phase during vapor-liquid phase mass transfer, and meanwhile, nonvolatile components in the vapor phase are transferred into the liquid phase.
The further improvement lies in that: in the third step, the volume of the enamel acid tank is 1 cubic meter, the acid washing reaction of the distillate and the acid solution is carried out at normal temperature and normal pressure, the reaction time is 1 hour, and the acid solution is separated from the mixed solution and then is led into the enamel acid tank for recycling.
The further improvement lies in that: and in the third step, sampling and detecting the material after the material is pickled, and pickling the material again if the indexes of alkali substances and phenolic substances in the material have the height regulated threshold values.
The further improvement lies in that: in the third step and the fourth step, the acid solution is separated from the mixed solution and then is led into the enamel acid tank for recycling, the alkali solution is separated from the separating tank and then is led into the enamel alkali tank for recycling, and the acid solution and the alkali solution are discarded after being reused for 2 months.
The further improvement lies in that: the raw oil is oil field light oil, the acid solution is a concentrated sulfuric acid solution with the concentration of 98%, and the alkali solution is a sodium hydroxide solution with the concentration of 99%.
The invention has the beneficial effects that: the invention firstly heats and reacts raw oil to a rectification reaction state of vapor-liquid separation through a rectification tower, then prepares distillate and naphtha through condensation reflux, then the distillate is sequentially subjected to acid washing and alkali washing, and finally the high-purity industrial isohexane is prepared, compared with the traditional isohexane preparation process, the method has the characteristics of short production line, simple preparation equipment, easy operation, safe and stable preparation process and high yield, and the oil field light oil is used as raw oil, so that the raw material has wide and rich sources and low price, is suitable for large-scale production and preparation, reduces the preparation cost to a certain extent, reduces the energy consumption, the pollution degree to the environment is small, the environment is protected and safe, in addition, the obtained naphtha can be used as chemical raw materials for external sales, thereby improving the comprehensive utilization rate of the raw oil, bringing excellent economic benefit and being worth of wide popularization.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flow chart of the manufacturing process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," "fourth," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1, this example provides a process for preparing isohexane, comprising the following steps:
the method comprises the following steps: raw material vapor-liquid separation
Raw oil is pumped into a reactor at the bottom of a rectifying tower through a raw material pump, the raw oil is heated to react, materials in the reactor form a gas-liquid state after being heated for a specified time, and the raw oil enters a rectifying reaction state, the raw oil is oil field light oil, wherein a heating source of the raw oil adopts high-temperature vacuum generated by a coal-fired steam boiler, the heating temperature in the reactor is controlled to be 80-90 ℃, and the heating reaction time is more than 5 hours;
step two: distillate preparation
According to the first step, firstly, condensing steam in materials in a rectifying tower through a condenser and refluxing the steam to a reflux tank to enable the steam and the liquid in the materials to be in countercurrent contact and realize interphase mass transfer to obtain high-purity volatile tower top distillate and high-purity difficultly-volatile tower bottom sediment, then guiding the distillate into a semi-finished product tank for temporary storage and standby application, guiding the tower bottom sediment into a storage tank for storage to obtain naphtha for sale, selecting the number of times of condensation reaction according to the purity of the materials required by production in the condensation process, allowing volatile components in a liquid phase to enter a gas phase during the vapor-liquid interphase mass transfer, and simultaneously transferring the difficultly-volatile components in the vapor phase into the liquid phase;
step three: acid pickling materials
According to the second step, firstly, placing acid solution with specified weight part into an enamel acid tank, then guiding distillate in a semi-finished product tank into the enamel acid tank and carrying out acid washing reaction with the acid solution, removing alkaline impurities and phenolic substances in the distillate, guiding mixed solution into a settling tank after the acid washing reaction is finished, and separating the material from the acid solution to obtain the acid-washed material, wherein the volume of the enamel acid tank is 1 cubic meter, the acid washing reaction of the distillate and the acid solution is carried out at normal temperature and normal pressure, the reaction time is 1 hour, the acid solution is separated from the mixed solution and then is guided into the enamel acid tank for recycling, the material is subjected to sampling detection after acid washing, if the indexes of the alkaline substances and the phenolic substances in the material are high and specified threshold values, the acid solution is concentrated sulfuric acid solution with the concentration of 98%, the acid solution is separated from the mixed solution and then is guided into the acid tank for recycling, and scrapped after being used repeatedly for 2 months;
step four: preparation of finished product
According to the third step, firstly putting alkali solution with specified weight part into an enamel alkali tank, then introducing the material after acid washing into the enamel alkali tank and carrying out alkali washing reaction with the alkali solution, removing acid impurities in the material, introducing the reaction solution into a separation tank after the alkali washing reaction is finished, separating the material from the alkali solution to obtain the material after alkali washing, then introducing the material after alkali washing into a finished product storage tank to obtain high-purity process isohexane, wherein the alkali solution is sodium hydroxide solution with the concentration of 99%, and after the alkali solution is separated from the separation tank, the alkali solution is introduced into the enamel alkali tank again for recycling and is discarded after being reused for 2 months.
The isohexane preparation process comprises the steps of heating and reacting raw oil to a rectification reaction state of vapor-liquid separation through a rectification tower, preparing distillate and naphtha through cold condensation reflux, and then sequentially carrying out acid washing and alkali washing on the distillate to finally prepare the high-purity industrial isohexane, compared with the traditional isohexane preparation process, the process has the characteristics of short production line, simple preparation equipment, easy operation, safe and stable preparation process and high yield, and the light oil of an oil field is used as the raw oil, so that the raw material has wide and rich sources and low price, is suitable for large-scale production preparation, reduces the preparation cost to a certain extent, reduces the energy consumption, has small pollution degree to the environment, is environment-friendly and safe, and in addition, the obtained naphtha can be used as a chemical raw material for export sales, thereby improving the comprehensive utilization rate of the raw oil and bringing excellent economic benefits, is worthy of wide popularization.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (7)

1. A process for preparing isohexane is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: raw material vapor-liquid separation
Raw oil is pumped into a reactor at the bottom of a rectifying tower through a raw material pump, the raw oil is heated to react, and after the raw oil is heated for a specified time, materials in the reactor form a vapor-liquid state and enter a rectifying reaction state;
step two: distillate preparation
According to the first step, firstly, condensing steam in the materials in the rectifying tower through a condenser and refluxing the steam to a reflux tank to enable the steam-liquid two phases in the materials to be in countercurrent contact and realize interphase mass transfer to obtain high-purity volatile tower top distillate and high-purity nonvolatile tower bottom sediment, then guiding the distillate into a semi-finished product tank for temporary storage and standby application, and guiding the tower bottom sediment into a storage tank for storage to obtain naphtha for sale;
step three: acid pickling materials
According to the second step, firstly, putting acid solution with specified weight part into an enamel acid tank, then guiding distillate in a semi-finished product tank into the enamel acid tank and carrying out acid washing reaction with the acid solution, removing alkaline impurities and phenolic substances in the distillate, guiding mixed solution into a settling tank after the acid washing reaction is finished, and separating the materials from the acid solution to obtain the acid-washed materials;
step four: preparation of finished product
According to the third step, firstly, putting alkali solution with specified weight part into an enamel alkali tank, then introducing the material after acid washing into the enamel alkali tank and carrying out alkali washing reaction with the alkali solution, removing acid impurities in the material, introducing the reaction solution into a separation tank after the alkali washing reaction is finished, separating the material from the alkali solution to obtain the material after alkali washing, and then introducing the material after alkali washing into a finished product storage tank to obtain high-purity process isohexane.
2. The process of claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: in the first step, the raw oil heating source adopts high-temperature vacuum gas generated by a coal-fired steam boiler, the heating temperature in the reactor is controlled to be 80-90 ℃, and the heating reaction time is longer than 5 hours.
3. The process of claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: in the second step, the condensation reaction times are selected according to the purity of the materials required by production in the condensation process, volatile components in the liquid phase enter the gas phase during vapor-liquid phase mass transfer, and meanwhile, nonvolatile components in the vapor phase are transferred into the liquid phase.
4. The process of claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: in the third step, the volume of the enamel acid tank is 1 cubic meter, the acid washing reaction of the distillate and the acid solution is carried out at normal temperature and normal pressure, the reaction time is 1 hour, and the acid solution is separated from the mixed solution and then is led into the enamel acid tank for recycling.
5. The process of claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: and in the third step, sampling and detecting the material after the material is pickled, and pickling the material again if the indexes of alkali substances and phenolic substances in the material have the height regulated threshold values.
6. The process of claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: in the third step and the fourth step, the acid solution is separated from the mixed solution and then is led into the enamel acid tank for recycling, the alkali solution is separated from the separating tank and then is led into the enamel alkali tank for recycling, and the acid solution and the alkali solution are discarded after being reused for 2 months.
7. The process of claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: the raw oil is oil field light oil, the acid solution is a concentrated sulfuric acid solution with the concentration of 98%, and the alkali solution is a sodium hydroxide solution with the concentration of 99%.
CN202110241167.7A 2021-03-04 2021-03-04 Isohexane preparation process Pending CN113004112A (en)

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Application Number Priority Date Filing Date Title
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB639137A (en) * 1947-04-24 1950-06-21 Midland Tar Distillers Ltd Improvements relating to the refining of naptha produced by the distillation of coaltar
CN1342630A (en) * 2000-09-12 2002-04-03 李季 Process for preparing high-purity n-pentane
CN101875594A (en) * 2009-04-30 2010-11-03 中国海洋石油总公司 Method for preparing narrow fraction nontoxic high-purity isohexane
CN102675023A (en) * 2012-05-19 2012-09-19 淄博汇佳橡胶新型材料有限公司 Preparation method of narrow-fraction high-purity isohexane
CN103833499A (en) * 2012-11-27 2014-06-04 中国石油天然气股份有限公司 Method for preparing high-purity isohexane solvent oil
CN107602329A (en) * 2017-09-15 2018-01-19 江苏科力特环保科技有限公司 A kind of recovery process of solvent hexamethylene
CN109160870A (en) * 2018-09-14 2019-01-08 成都市科隆化学品有限公司 A kind of production method of chromatograph-grade normal heptane
CN110668909A (en) * 2019-10-23 2020-01-10 成都市科隆化学品有限公司 Purification method of environment-friendly n-hexane

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB639137A (en) * 1947-04-24 1950-06-21 Midland Tar Distillers Ltd Improvements relating to the refining of naptha produced by the distillation of coaltar
CN1342630A (en) * 2000-09-12 2002-04-03 李季 Process for preparing high-purity n-pentane
CN101875594A (en) * 2009-04-30 2010-11-03 中国海洋石油总公司 Method for preparing narrow fraction nontoxic high-purity isohexane
CN102675023A (en) * 2012-05-19 2012-09-19 淄博汇佳橡胶新型材料有限公司 Preparation method of narrow-fraction high-purity isohexane
CN103833499A (en) * 2012-11-27 2014-06-04 中国石油天然气股份有限公司 Method for preparing high-purity isohexane solvent oil
CN107602329A (en) * 2017-09-15 2018-01-19 江苏科力特环保科技有限公司 A kind of recovery process of solvent hexamethylene
CN109160870A (en) * 2018-09-14 2019-01-08 成都市科隆化学品有限公司 A kind of production method of chromatograph-grade normal heptane
CN110668909A (en) * 2019-10-23 2020-01-10 成都市科隆化学品有限公司 Purification method of environment-friendly n-hexane

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