CN114471482A - Preparation method and application of adsorbent for reducing water content in oil product - Google Patents

Preparation method and application of adsorbent for reducing water content in oil product Download PDF

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CN114471482A
CN114471482A CN202011149924.XA CN202011149924A CN114471482A CN 114471482 A CN114471482 A CN 114471482A CN 202011149924 A CN202011149924 A CN 202011149924A CN 114471482 A CN114471482 A CN 114471482A
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adsorbent
water content
drying
preparation
oil product
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Chinese (zh)
Inventor
刘乃旺
孟繁羽
孟璇
施力
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East China University of Science and Technology
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East China University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12—Naturally occurring clays or bleaching earth
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
    • C10G25/003—Specific sorbent material, not covered by C10G25/02 or C10G25/03
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G33/00—Dewatering or demulsification of hydrocarbon oils
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

The invention relates to a preparation method of an adsorbent for reducing the water content of an oil product, and particularly provides an adsorbent for removing trace water in the oil product; the adsorbent is prepared by the following steps: (1) at room temperature 25oC, mixing food-grade sodium polyacrylate resin and activated clay under the normal pressure condition, and dripping deionized water to assist the formation of the adsorbent; (2) drying after molding to obtain an adsorbent precursor; (3) and (5) washing the adsorbent precursor by using an alcohol solution, and drying to obtain the adsorbent. In the present invention, the adsorbent exhibits good adsorption performance. The invention also relates to the adsorbent for reducing the water content of the oil product, which is obtained by the preparation method. The invention also provides the aboveThe application of the adsorbent in reducing the water content of oil products.

Description

Preparation method and application of adsorbent for reducing water content in oil product
Technical Field
The invention relates to an adsorbent technology for reducing water content in oil products, in particular to an adsorbent for reducing water content in oil products and a preparation method and application thereof.
Background
In recent years, with the rapid development of crude oil refining industry in China and the vigorous intervention of civil enterprises, the demand of diesel oil is continuously increased. The light diesel oil in the catalytic diesel oil stripping tower is stripped through steam, so that the flash point of the light diesel oil is improved, the gasoline yield is improved, the stripping working principle is simple, and the application in the diesel oil production process is relatively common. However, the process often results in higher water content of the diesel oil, and the overhigh water content of the diesel oil prolongs the settling time of the diesel oil in the tank field, further influences the subsequent processing and blending of the diesel oil and is not beneficial to the stable production of the device. Saturated salt water is generated by a sodium chloride salt tank so as to reduce the water content in the diesel oil, which is an experience method generally adopted in the initial stage of the oil refining industry in China, although the method has a certain effect, a large amount of chloride ions are introduced into oil products, and the method causes corrosion harm to the subsequent storage and use of the diesel oil to a certain extent. In order to ensure the quality of oil products, various adsorbents are actively developed for the fixed bed oil product dehydration process.
The adsorbents commonly used in industry mainly include activated carbon, activated alumina, silica gel, molecular sieves, and the like. The active carbon has large surface area and rich pore channels, but the adsorption is not selective, and the adsorption of the diesel oil can occupy a large number of adsorption sites, so that the removal of trace water in the oil product is not ideal; the water absorption of alumina and silica gel is about 15% generally, and the alumina and silica gel are often used for the dehydration of small-quantity fine chemicals; the molecular sieve, represented by A-type molecular sieve, has water absorption of about 15-20%, and is mainly used for drying low-carbon hydrocarbon due to small pore diameter. The dehydrating agent seems to be simple, but if the dehydrating agent can be successfully developed, the dehydrating agent has cost advantage, can be used for fine dehydrating adsorbent of bulk chemicals, still has wide application prospect, has obvious effect on improving product quality, and is simultaneously beneficial to reducing the discharge of sodium chloride waste liquid and reducing the environmental protection pressure of a workshop.
The diesel oil refining process usually adopts a steam stripping tower to remove a small amount of hydrogen sulfide and dry gas in the diesel oil. In practical production application, the diesel oil after steam stripping in most refineries has the condition of 'haziness', and the appearance is turbid and not bright, so that the product delivery is influenced. The phenomenon of fogging is caused by the fact that a small amount of water is dissolved and suspended in the diesel oil, so that the appearance of the diesel oil looks cloudy. If the amount of water is small and the water droplets are relatively large, the fuel may appear to be "mist". The smaller the water droplets, the easier they are suspended in the fuel and the longer they last, the more severe the emulsion is formed. Therefore, it is necessary to use a relatively general adsorbent to remove water from diesel fuel.
CN107345149A discloses a diesel oil dehydration method, which comprises the following steps: fully mixing the diesel oil containing emulsified water with alcohol or alcohol amine solvent according to a certain proportion; standing the mixed solution for a period of time: the upper layer of the standing solution is clear diesel oil, and the lower layer is aqueous alcohol or alcohol amine solvent. The method needs more organic solvent, is not economical and environment-friendly, and also needs subsequent treatment on the solvent.
CN1903829A discloses a dehydration process of isooctyl nitrate, the carbon skeleton is further in the technical field of carbon and nitrogen-containing compounds substituted by singly-bonded oxygen atoms, the dehydration process comprises the steps of separating most of water by sedimentation, and separating trace water by anhydrous sodium sulfate. The water content in the finished product of the method is controlled to be 0.01 percent and can not reach the ppm level.
Disclosure of Invention
In order to solve the problems of poor dehydration effect of the adsorbent, environmental pollution of a prepared reagent and the like in the prior art, the invention aims to provide the adsorbent for reducing the water content of diesel oil and the preparation method and application thereof.
The invention provides a preparation method of an adsorbent for reducing the water content of oil in an oil product, which comprises the following steps: s1, mixing activated clay with a certain mass and sodium polyacrylate resin accounting for 1% -30% of the mass of the activated clay monomer, and dripping deionized water to assist the formation of the adsorbent; s2, drying after molding to obtain an adsorbent precursor; and S3, washing the adsorbent precursor in an alcohol solution, filtering and drying to obtain the adsorbent.
The step S1 specifically includes: taking a certain mass of activated clay, uniformly mixing sodium polyacrylate resin accounting for 1-30% of the mass of the activated clay monomer, and dripping deionized water to assist the adsorbent in extruding strips or tabletting for forming.
The step S2 specifically includes: drying at 80-120 ℃ after molding to obtain the adsorbent precursor.
The step S3 specifically includes: and (3) washing the adsorbent precursor in an alcohol solution, filtering, and drying at 80 ℃ to obtain the adsorbent.
The invention also provides the adsorbent for reducing the water content of the diesel oil, which is obtained by the preparation method.
The invention also provides application of the adsorbent in reducing the water content of diesel oil.
The adsorbent provided by the invention takes activated clay as a carrier, and sodium polyacrylate resin is used for modifying the adsorbent to obtain the solid adsorbent capable of efficiently absorbing water. Experiments show that the adsorbent has long service life, and still has higher activity after 5 times of inactivation regeneration cycles, so the defects of the existing adsorbent can be obviously improved, and the adsorbent has wide industrial application prospects. Compared with a common salt dehydration process and a 5A molecular sieve dehydration process which are adopted for reducing the water content in the materials in the production of diesel oil, the common salt has adverse effects of easy corrosion of pipelines, large amount of waste liquid discharge and the like due to the existence of chloride ions; the 5A molecular sieve has weak water absorption and oil absorption selectivity, can effectively replace salt and the 5A molecular sieve, is favorable for protecting refinery equipment, and can reduce the discharge of waste water, reduce the maintenance cost and improve the green production level of enterprises for the refining enterprises.
Detailed Description
The present invention is described by the following examples, but the present invention is not limited to the following examples, and variations and implementations are included in the technical scope of the present invention without departing from the spirit of the invention described above and below. The present invention will be further described with reference to the following specific examples.
Example 1
Uniformly mixing activated clay with a certain mass, sodium polyacrylate resin accounting for 3% of the mass of the activated clay monomer, dropwise adding deionized water to assist the adsorbent in extruding strips for forming, and drying at 80 ℃ for 24 hours after forming to obtain an adsorbent precursor. And (3) washing the adsorbent precursor in an alcohol solution, filtering, and drying for 24 hours at 80 ℃ to obtain the adsorbent A.
Example 2
Taking activated clay with a certain mass, uniformly mixing sodium polyacrylate resin with 5% of the mass of the activated clay monomer, dropwise adding deionized water to assist the adsorbent in extruding and molding strips, and drying for 24 hours at 80 ℃ after molding to obtain an adsorbent precursor. And (3) washing the adsorbent precursor in an alcohol solution, filtering, and drying for 24 hours at 80 ℃ to obtain an adsorbent B.
Example 3
Uniformly mixing activated clay with a certain mass, sodium polyacrylate resin with the mass being 7% of that of activated clay monomer, dripping deionized water to assist the adsorbent in extruding and molding, and drying for 24 hours at 80 ℃ after molding to obtain an adsorbent precursor. And (3) washing the adsorbent precursor in an alcohol solution, filtering, and drying for 24 hours at 80 ℃ to obtain the adsorbent C.
Example 4
Uniformly mixing activated clay with a certain mass, sodium polyacrylate resin accounting for 10% of the mass of the activated clay monomer, dropwise adding deionized water to assist the adsorbent in extruding strips for forming, and drying at 80 ℃ for 24 hours after forming to obtain an adsorbent precursor. And (3) washing the adsorbent precursor in an alcohol solution, filtering, and drying for 24 hours at 80 ℃ to obtain the adsorbent D.
Example 5
Uniformly mixing activated clay with a certain mass, 20% of sodium polyacrylate resin relative to the mass of activated clay monomers, dropwise adding deionized water to assist the adsorbent in extruding and molding, and drying for 24 hours at 80 ℃ after molding to obtain an adsorbent precursor. And (3) washing the adsorbent precursor in an alcohol solution, filtering, and drying for 24 hours at 80 ℃ to obtain the adsorbent E.
Example 6
Uniformly mixing activated clay with a certain mass, sodium polyacrylate resin accounting for 30% of the mass of the activated clay monomer, dropwise adding deionized water to assist the adsorbent in extruding strips for forming, and drying at 80 ℃ for 24 hours after forming to obtain an adsorbent precursor. And (3) washing the adsorbent precursor in an alcohol solution, filtering, and drying for 24 hours at 80 ℃ to obtain the adsorbent F.
Example 7
The adsorbent A, B, C in examples 1, 2 and 3 was taken out after the activity test was completed, and was dried at 80 ℃ for 24 hours after being washed with an alcohol solution, thereby realizing the regeneration of the adsorbent A, B, C. Adsorbent G, H, I was obtained after 5 cycles of deactivation regeneration.
Example 8
The experiment for removing trace moisture in diesel oil is carried out in a micro fixed bed reactor. The reaction conditions were as follows: the procedure of example 4 was repeatedThe additive D and the quartz sand are put into a reactor in a certain order at normal temperature and pressure with a mass space velocity of 13.36h-1The moisture content of the sample at the 3 rd hour was analyzed by a Karl Fischer moisture meter. The 5A molecular sieve is a common adsorbent for removing water in a refinery, the argil is a main component of the adsorbent, and in order to illustrate the effect of the novel adsorbent, the 5A molecular sieve and the argil are used as comparison, and the dehydration performance test of the 5A molecular sieve and the argil is carried out under the same condition.
The water absorption rate X of the adsorbent is equal to [ (raw oil water content-discharged oil water content)/raw oil water content ]. 100%, and the raw oil water content is 55.1ppm/g oil.
The catalytic activity of the corresponding adsorbents for each example is shown in table 1 below:
TABLE 1
Figure BDA0002740862320000041
Example 9
The static adsorption experiment for removing trace moisture in the aromatic hydrocarbon material is carried out in a sealed container. The reaction conditions were as follows: the adsorbents A to I of examples 1 to 7 and the aromatic hydrocarbon material were placed in a sealed container at a solvent-oil ratio of 1:20, and a sample after 24 hours of adsorption was taken and analyzed for moisture content with a Karl Fischer moisture meter at normal temperature and pressure. The 5A molecular sieve is an adsorbent for removing water commonly used in refineries, the argil is a main component of the adsorbent, and in order to illustrate the effect of the novel adsorbent, the 5A molecular sieve and the argil are used for comparison, and the dehydration performance test of the 5A molecular sieve and the argil is carried out under the same condition.
The water absorption of the adsorbent X ═ [ (water content of the raw oil-water content of the discharged oil)/water content of the raw oil ]. 100%, and the water content of the raw oil is 350.9ppm/g oil. The organic composition of the feed oil is shown in the following table 2:
TABLE 2
Figure BDA0002740862320000042
The catalytic activity of the corresponding adsorbents for each example is shown in table 3 below:
TABLE 3
Figure BDA0002740862320000043
Figure BDA0002740862320000051
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.

Claims (6)

1. The preparation method of the adsorbent for reducing the water content in the oil product is characterized by comprising the following steps of:
s1, mixing activated clay with a certain mass and sodium polyacrylate resin with a certain proportion relative to the mass of activated clay monomers, and dripping deionized water to assist the formation of the adsorbent;
s2, drying after molding to obtain an adsorbent precursor; and
and S3, washing the adsorbent precursor in an alcohol solution, filtering and drying to obtain the adsorbent.
2. The preparation method according to claim 1, wherein the step S1 specifically comprises: taking a certain mass of activated clay, uniformly mixing sodium polyacrylate resin accounting for 1-30% of the mass of the activated clay monomer, and dripping deionized water to assist the adsorbent in extruding strips or tabletting for forming.
3. The preparation method according to claim 1, wherein the step S2 specifically comprises: after molding 80oAnd C, drying to obtain the adsorbent precursor.
4. The preparation method according to claim 1, wherein the step S3 specifically comprises: washing adsorbent precursor in alcohol solution, filtering, and passing through 80-120oAnd C, drying to obtain the adsorbent.
5. An adsorbent for reducing water content of an oil product obtained by the method of any one of claims 1 to 4.
6. Use of the adsorbent according to claims 1-5 for reducing the water content in an oil product.
CN202011149924.XA 2020-10-23 2020-10-23 Preparation method and application of adsorbent for reducing water content in oil product Pending CN114471482A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1762577A (en) * 2005-09-28 2006-04-26 王傲乾 Tar absorption dehydration purifier
CN1903990A (en) * 2006-07-27 2007-01-31 宁守俭 Deacidification adsorbent for oil products and preparation method thereof
CN101270319A (en) * 2008-04-29 2008-09-24 长春理工大学 Room temperature dehydration method for hogwash oil with high-water uptake resin
US20150273433A1 (en) * 2012-10-03 2015-10-01 Nippon Shokubai Co., Ltd. Water absorbing agent and method for producing the same
CN107345149A (en) * 2016-05-05 2017-11-14 中国石化扬子石油化工有限公司 The removal methods of emulsified water in a kind of diesel oil
CN107937018A (en) * 2017-10-25 2018-04-20 马鞍山拓锐金属表面技术有限公司 A kind of preparation method of molecular sieve type Coal tar dehydrant

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1762577A (en) * 2005-09-28 2006-04-26 王傲乾 Tar absorption dehydration purifier
CN1903990A (en) * 2006-07-27 2007-01-31 宁守俭 Deacidification adsorbent for oil products and preparation method thereof
CN101270319A (en) * 2008-04-29 2008-09-24 长春理工大学 Room temperature dehydration method for hogwash oil with high-water uptake resin
US20150273433A1 (en) * 2012-10-03 2015-10-01 Nippon Shokubai Co., Ltd. Water absorbing agent and method for producing the same
CN107345149A (en) * 2016-05-05 2017-11-14 中国石化扬子石油化工有限公司 The removal methods of emulsified water in a kind of diesel oil
CN107937018A (en) * 2017-10-25 2018-04-20 马鞍山拓锐金属表面技术有限公司 A kind of preparation method of molecular sieve type Coal tar dehydrant

Non-Patent Citations (1)

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Title
詹益兴等: "《精细化工新产品（第1集）》", vol. 1, 科学技术文献出版社, pages: 123 *

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