CN109504160B - Preparation method of environment-friendly aromatic solvent for high-grade printing oil - Google Patents
Preparation method of environment-friendly aromatic solvent for high-grade printing oil Download PDFInfo
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- CN109504160B CN109504160B CN201811382708.2A CN201811382708A CN109504160B CN 109504160 B CN109504160 B CN 109504160B CN 201811382708 A CN201811382708 A CN 201811382708A CN 109504160 B CN109504160 B CN 109504160B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
Abstract
The invention discloses a preparation method of an environment-friendly aromatic solvent for high-grade printing oil, which specifically comprises the following steps: firstly, preparing porous fiber, and then sequentially carrying out acidification and silane coupling agent crosslinking treatment on the porous fiber to prepare crosslinked porous fiber; then adding the crosslinked porous fiber into a palladium acetate solution, introducing ammonia water, reacting and calcining under certain conditions to prepare a porous fiber crosslinking modified hydrogenation catalyst; adding the cracked C10 fraction into a hydrogenation reactor filled with a catalyst for hydrogenation reaction to prepare hydrogenated oil; and adding the prepared hydrogenated oil into a rectifying tower for vacuum rectification, and collecting fractions at the temperature of 165-185 ℃ and 190-220 ℃ to prepare the environment-friendly aromatic hydrocarbon solvent. The method has the advantages of simple operation, low cost, low sulfur content of the prepared aromatic hydrocarbon solvent and high yield.
Description
Technical Field
The invention relates to a preparation method of a solvent, in particular to a preparation method of an environment-friendly aromatic solvent for high-grade printing oil.
Background
The ink is a uniform mixture composed of color bodies (such as pigments, dyes and the like), binders, filling materials, additives and the like; printing can be carried out, and drying is carried out on the printed body; is a colored pasty adhesive with certain fluidity. Thus, color (hue), body (rheology such as thickness, fluidity, etc.) and drying properties are the three most important properties of the ink. They are of various types, have different physical properties, and are thick and sticky; while some are quite rare. Some vegetable oil is used as a vehicle; some uses resin and solvent or water as the binder. These are determined according to the object to be printed, i.e., the substrate, the printing method, the type of printing plate, the drying method, and the like. The solvent is used for printing a part of the printing ink, and the key for developing the printing ink with excellent performance is to prepare the environment-friendly printing ink with high melting point.
Chinese patent (201010110722.4) discloses a green environment-friendly composite solvent for printing ink and a preparation method thereof, the method adopts carbonyl oxidation to synthesize dimethyl carbonate and diethyl carbonate, the reaction products are respectively rectified and collected to obtain 90-94 ℃ fraction and 125-128 ℃ fraction, and finally the dimethyl carbonate, the diethyl carbonate, ethyl acetate, butyl acetate and cyclohexane are dispersed and adjusted to be uniform according to a certain volume ratio to obtain the product. The solvent prepared by the method has narrow distillation range, low aromatic hydrocarbon content, good solubility to resin and higher preparation cost.
Disclosure of Invention
The invention aims to provide a preparation method of an environment-friendly aromatic solvent for high-grade printing oil, aiming at the defects of the prior art, and the method has low requirements on equipment, and the prepared solvent has good storage stability, high boiling point, high yield and high purity.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an environment-friendly aromatic solvent for high-grade printing oil comprises the following steps:
(1) dissolving polyurethane in absolute ethyl alcohol to prepare a polyurethane solution; adding tetraethoxysilane, aluminum isopropoxide and ethyl acetate, stirring and mixing, preparing a fiber precursor from the prepared mixed solution by a filamentation process, placing the fiber precursor in a muffle furnace, and sintering for 1-4 hours under inert gas to prepare porous fiber;
(2) placing the prepared porous fiber in a nitric acid solution for light-proof dipping treatment for 10-20h, filtering, cleaning the porous fiber to be neutral by using deionized water, and drying to prepare pretreated porous fiber;
(3) adding the pretreated porous fiber into an ethanol solution of a silane coupling agent, slowly heating to 60-70 ℃, stirring, refluxing and reacting for 2-4h, cooling to room temperature after the reaction is finished, filtering, and drying to obtain the crosslinked porous fiber;
(4) dissolving palladium acetate in acetic acid to prepare a palladium acetate solution, adding the prepared crosslinked porous fiber, stirring for 1-3h at 30-40 ℃, adding an ammonia water solution, stirring for reaction for 4-9h at normal temperature after dropwise addition, filtering, drying, and sintering the dried solid in a muffle furnace at 550-750 ℃ for 3-5h to prepare a porous fiber crosslinking modified hydrogenation catalyst;
(5) adding the cracking C10 fraction into a hydrogenation reactor, wherein the hydrogen pressure is 4-8MPa, the hydrogen-oil volume ratio is 500-800, and the volume space velocity is 13-14.5h-1Carrying out hydrogenation reaction under the condition of (1) to prepare hydrogenated oil;
(6) and adding the prepared hydrogenated oil into a rectifying tower for vacuum rectification, and collecting fractions at the temperature of 165-185 ℃ and 190-220 ℃ to prepare the environment-friendly aromatic hydrocarbon solvent.
Preferably, in the step (1), the ratio of the polyurethane to the absolute ethyl alcohol to the amount of ethyl orthosilicate to the amount of aluminum isopropoxide to the amount of ethyl acetate is 1 g: 30mL of: (0.5-1) mL: (0.033-0.045) g: 1 mL.
Preferably, in the step (1), the temperature of the sintering treatment is 300-400 ℃.
Preferably, in the step (2), the ratio of the amount of the porous fiber to the nitric acid solution is 1 g: (50-60) mL.
Preferably, in the step (3), the ratio of the amount of the pretreated porous fiber to the amount of the silane coupling agent is 1 g: (0.01-0.05) mL.
Preferably, in the step (4), the mass concentration of the palladium acetate solution is 15 to 22%.
Preferably, in the step (4), the mass ratio of the palladium acetate to the crosslinked porous fibers is 1: (3-6).
As the optimization of the technical scheme, in the step (5), the temperature of the hydrogenation reaction is 130-160 ℃.
Preferably, in the step (5), the mass ratio of the cracked C10 fraction to the catalyst is (15-22): 0.3.
the invention has the following beneficial effects:
the method adopts catalytic hydrogenation and rectification to process and crack C10 fraction in a segmented manner, so that the yield of the environment-friendly aromatic solvent can be effectively improved; in the catalytic hydrogenation stage, firstly, a porous fiber precursor is prepared by filamentation of a mixed solution of polyurethane, tetraethoxysilane and aluminum isopropoxide, and then porous fibers are prepared by treatment under certain conditions, wherein the porous fibers are composite fibers of porous silicon oxide and porous aluminum oxide, and have high porosity and good mechanical properties;
according to the invention, the prepared porous fiber is sequentially treated by acid and silane coupling agent to prepare the crosslinked porous fiber, and the crosslinked porous fiber is placed in a palladium acetate solution, so that palladium ions can be effectively adsorbed in pores, uniform precipitation is carried out in the presence of ammonia water, and the prepared palladium oxide is uniformly dispersed in the pores of the porous fiber; the prepared catalyst can be fully contacted with the raw materials; thereby improving the yield of the environment-friendly solvent.
Detailed Description
In order to better understand the present invention, the following examples further illustrate the invention, the examples are only used for explaining the invention, not to constitute any limitation of the invention.
Example 1
A preparation method of an environment-friendly aromatic solvent for high-grade printing oil comprises the following steps:
(1) dissolving polyurethane in absolute ethyl alcohol to prepare a polyurethane solution; then adding tetraethoxysilane, aluminum isopropoxide and ethyl acetate, stirring and mixing, preparing a fiber precursor from the prepared mixed solution by a filamentation process, placing the fiber precursor in a muffle furnace, and sintering for 1h at the temperature of 300-400 ℃ under inert gas to prepare porous fiber; wherein the dosage ratio of the polyurethane to the absolute ethyl alcohol to the tetraethoxysilane to the aluminum isopropoxide to the ethyl acetate is 1 g: 30mL of: 0.5 mL: 0.033 g: 1 mL;
(2) placing the prepared porous fiber in a nitric acid solution for light-proof dipping treatment for 10 hours, filtering, cleaning the porous fiber to be neutral by adopting deionized water, and drying to prepare pretreated porous fiber;
(3) adding the pretreated porous fiber into an ethanol solution of a silane coupling agent, slowly heating to 60-70 ℃, stirring, refluxing, reacting for 2 hours, cooling to room temperature after the reaction is finished, filtering, and drying to obtain the crosslinked porous fiber; wherein the dosage ratio of the pretreated porous fiber to the silane coupling agent is 1 g: 0.01 mL;
(4) dissolving palladium acetate in acetic acid to prepare a palladium acetate solution with the mass concentration of 15%, adding the prepared crosslinked porous fiber, stirring at 30-40 ℃ for 1h, adding an ammonia water solution, stirring at normal temperature for reaction for 4h after dropwise addition, filtering, drying, and sintering the dried solid in a muffle furnace at 550 ℃ for 3h to prepare the porous fiber crosslinking modified hydrogenation catalyst; wherein the mass ratio of the palladium acetate to the cross-linked porous fiber is 1: 3;
(5) adding the cracked C10 fraction into a hydrogenation reactor, and adding hydrogen oil under the hydrogen pressure of 4-8MPaThe volume ratio is 500-800, the volume space velocity is 13-14.5h-1Hydrogenation reaction is carried out at the temperature of 130 ℃ to prepare hydrogenated oil; wherein the mass ratio of the cracking C10 fraction to the catalyst is 15: 0.3;
(6) and adding the prepared hydrogenated oil into a rectifying tower for vacuum rectification, and collecting fractions at the temperature of 165-185 ℃ and 190-220 ℃ to prepare the environment-friendly aromatic hydrocarbon solvent.
Example 2
A preparation method of an environment-friendly aromatic solvent for high-grade printing oil comprises the following steps:
(1) dissolving polyurethane in absolute ethyl alcohol to prepare a polyurethane solution; then adding tetraethoxysilane, aluminum isopropoxide and ethyl acetate, stirring and mixing, preparing a fiber precursor from the prepared mixed solution by a filamentation process, placing the fiber precursor in a muffle furnace, and sintering for 4 hours at the temperature of 300-400 ℃ under inert gas to prepare porous fiber; wherein the dosage ratio of the polyurethane to the absolute ethyl alcohol to the tetraethoxysilane to the aluminum isopropoxide to the ethyl acetate is 1 g: 30mL of: 1mL of: 0.045 g: 1 mL;
(2) placing the prepared porous fiber in a nitric acid solution for light-proof dipping treatment for 20h, filtering, cleaning the porous fiber to be neutral by using deionized water, and drying to obtain pretreated porous fiber;
(3) adding the pretreated porous fiber into an ethanol solution of a silane coupling agent, slowly heating to 60-70 ℃, stirring, refluxing, reacting for 4 hours, cooling to room temperature after the reaction is finished, filtering, and drying to obtain the crosslinked porous fiber; wherein the dosage ratio of the pretreated porous fiber to the silane coupling agent is 1 g: 0.05 mL;
(4) dissolving palladium acetate in acetic acid to prepare a palladium acetate solution with the mass concentration of 22%, adding the prepared crosslinked porous fiber, stirring for 3 hours at the temperature of 30-40 ℃, adding an ammonia water solution, stirring for reaction for 9 hours at normal temperature after dropwise addition, filtering, drying, and sintering the dried solid for 5 hours at the temperature of 750 ℃ in a muffle furnace to prepare the porous fiber crosslinked modified hydrogenation catalyst; wherein the mass ratio of the palladium acetate to the cross-linked porous fiber is 1: 6;
(5) adding cracked C10 fractionThe hydrogen pressure is 4-8MPa, the volume ratio of hydrogen to oil is 500-800, and the volume space velocity is 13-14.5h-1Hydrogenation reaction is carried out at the temperature of 160 ℃ to prepare hydrogenated oil; wherein the mass ratio of the cracking C10 fraction to the catalyst is 22: 0.3;
(6) and adding the prepared hydrogenated oil into a rectifying tower for vacuum rectification, and collecting fractions at the temperature of 165-185 ℃ and 190-220 ℃ to prepare the environment-friendly aromatic hydrocarbon solvent.
Example 3
A preparation method of an environment-friendly aromatic solvent for high-grade printing oil comprises the following steps:
(1) dissolving polyurethane in absolute ethyl alcohol to prepare a polyurethane solution; then adding tetraethoxysilane, aluminum isopropoxide and ethyl acetate, stirring and mixing, preparing a fiber precursor from the prepared mixed solution by a filamentation process, placing the fiber precursor in a muffle furnace, and sintering for 2 hours at the temperature of 300 ℃ and 400 ℃ under inert gas to prepare porous fiber; wherein the dosage ratio of the polyurethane to the absolute ethyl alcohol to the tetraethoxysilane to the aluminum isopropoxide to the ethyl acetate is 1 g: 30mL of: 0.6 mL: 0.035 g: 1 mL;
(2) placing the prepared porous fiber in a nitric acid solution for light-proof dipping treatment for 12h, filtering, cleaning the porous fiber to be neutral by adopting deionized water, and drying to obtain pretreated porous fiber;
(3) adding the pretreated porous fiber into an ethanol solution of a silane coupling agent, slowly heating to 60-70 ℃, stirring, refluxing, reacting for 2.5 hours, cooling to room temperature after the reaction is finished, filtering, and drying to obtain the crosslinked porous fiber; wherein the dosage ratio of the pretreated porous fiber to the silane coupling agent is 1 g: 0.02 mL;
(4) dissolving palladium acetate in acetic acid to prepare a palladium acetate solution with the mass concentration of 16%, adding the prepared crosslinked porous fiber, stirring at 30-40 ℃ for 1.5h, adding an ammonia water solution, stirring at normal temperature for reaction for 5h after dropwise addition, filtering, drying, and sintering the dried solid in a muffle furnace at 550-750 ℃ for 3.5h to prepare the porous fiber crosslinking modified hydrogenation catalyst; wherein the mass ratio of the palladium acetate to the cross-linked porous fiber is 1: 4;
(5) adding the cracking C10 fraction into a hydrogenation reactor, wherein the hydrogen pressure is 4-8MPa, the hydrogen-oil volume ratio is 500-800, and the volume space velocity is 13-14.5h-1Hydrogenation reaction is carried out at the temperature of 140 ℃ to prepare hydrogenated oil; wherein the mass ratio of the cracking C10 fraction to the catalyst is 17: 0.3;
(6) and adding the prepared hydrogenated oil into a rectifying tower for vacuum rectification, and collecting fractions at the temperature of 165-185 ℃ and 190-220 ℃ to prepare the environment-friendly aromatic hydrocarbon solvent.
Example 4
A preparation method of an environment-friendly aromatic solvent for high-grade printing oil comprises the following steps:
(1) dissolving polyurethane in absolute ethyl alcohol to prepare a polyurethane solution; then adding tetraethoxysilane, aluminum isopropoxide and ethyl acetate, stirring and mixing, preparing a fiber precursor from the prepared mixed solution by a filamentation process, placing the fiber precursor in a muffle furnace, and sintering at the temperature of 300-400 ℃ under inert gas for 2.5 hours to prepare porous fiber; wherein the dosage ratio of the polyurethane to the absolute ethyl alcohol to the tetraethoxysilane to the aluminum isopropoxide to the ethyl acetate is 1 g: 30mL of: 0.7 mL: 0.037 g: 1 mL;
(2) placing the prepared porous fiber in a nitric acid solution for light-proof dipping treatment for 14h, filtering, cleaning the porous fiber to be neutral by using deionized water, and drying to obtain pretreated porous fiber;
(3) adding the pretreated porous fiber into an ethanol solution of a silane coupling agent, slowly heating to 60-70 ℃, stirring, refluxing and reacting for 3 hours, cooling to room temperature after the reaction is finished, filtering, and drying to obtain the crosslinked porous fiber; wherein the dosage ratio of the pretreated porous fiber to the silane coupling agent is 1 g: 0.03 mL;
(4) dissolving palladium acetate in acetic acid to prepare a palladium acetate solution with the mass concentration of 18%, adding the prepared crosslinked porous fiber, stirring at 30-40 ℃ for 2h, adding an ammonia water solution, stirring at normal temperature for reaction for 6h after dropwise addition, filtering, drying, and sintering the dried solid in a muffle furnace at 550-750 ℃ for 4h to prepare the porous fiber crosslinked modified hydrogenation catalyst; wherein the mass ratio of the palladium acetate to the cross-linked porous fiber is 1: 4;
(5) adding the cracking C10 fraction into a hydrogenation reactor, wherein the hydrogen pressure is 4-8MPa, the hydrogen-oil volume ratio is 500-800, and the volume space velocity is 13-14.5h-1Hydrogenation reaction is carried out at the temperature of 140 ℃ to prepare hydrogenated oil; wherein the mass ratio of the cracking C10 fraction to the catalyst is 18: 0.3;
(6) and adding the prepared hydrogenated oil into a rectifying tower for vacuum rectification, and collecting fractions at the temperature of 165-185 ℃ and 190-220 ℃ to prepare the environment-friendly aromatic hydrocarbon solvent.
Example 5
A preparation method of an environment-friendly aromatic solvent for high-grade printing oil comprises the following steps:
(1) dissolving polyurethane in absolute ethyl alcohol to prepare a polyurethane solution; then adding tetraethoxysilane, aluminum isopropoxide and ethyl acetate, stirring and mixing, preparing a fiber precursor from the prepared mixed solution by a filamentation process, placing the fiber precursor in a muffle furnace, and sintering for 3 hours at the temperature of 300-400 ℃ under inert gas to prepare porous fiber; wherein the dosage ratio of the polyurethane to the absolute ethyl alcohol to the tetraethoxysilane to the aluminum isopropoxide to the ethyl acetate is 1 g: 30mL of: 0.8 mL: 0.039 g: 1 mL;
(2) placing the prepared porous fiber in a nitric acid solution for light-proof dipping treatment for 16h, filtering, cleaning the porous fiber to be neutral by using deionized water, and drying to obtain pretreated porous fiber;
(3) adding the pretreated porous fiber into an ethanol solution of a silane coupling agent, slowly heating to 60-70 ℃, stirring, refluxing and reacting for 3 hours, cooling to room temperature after the reaction is finished, filtering, and drying to obtain the crosslinked porous fiber; wherein the dosage ratio of the pretreated porous fiber to the silane coupling agent is 1 g: 0.04 mL;
(4) dissolving palladium acetate in acetic acid to prepare a palladium acetate solution with the mass concentration of 18%, adding the prepared crosslinked porous fiber, stirring at 30-40 ℃ for 2h, adding an ammonia solution, stirring at normal temperature for reaction for 7h after dropwise addition, filtering, drying, and sintering the dried solid at 550-750 ℃ in a muffle furnace for 4.5h to prepare the porous fiber crosslinked modified hydrogenation catalyst; wherein the mass ratio of the palladium acetate to the cross-linked porous fiber is 1: 5;
(5) adding the cracking C10 fraction into a hydrogenation reactor, wherein the hydrogen pressure is 4-8MPa, the hydrogen-oil volume ratio is 500-800, and the volume space velocity is 13-14.5h-1Hydrogenation reaction is carried out at the temperature of 150 ℃ to prepare hydrogenated oil; wherein the mass ratio of the cracking C10 fraction to the catalyst is 19: 0.3;
(6) and adding the prepared hydrogenated oil into a rectifying tower for vacuum rectification, and collecting fractions at the temperature of 165-185 ℃ and 190-220 ℃ to prepare the environment-friendly aromatic hydrocarbon solvent.
Example 6
A preparation method of an environment-friendly aromatic solvent for high-grade printing oil comprises the following steps:
(1) dissolving polyurethane in absolute ethyl alcohol to prepare a polyurethane solution; then adding tetraethoxysilane, aluminum isopropoxide and ethyl acetate, stirring and mixing, preparing a fiber precursor from the prepared mixed solution by a filamentation process, placing the fiber precursor in a muffle furnace, and sintering at the temperature of 300-400 ℃ under inert gas for 3.5 hours to prepare porous fiber; wherein the dosage ratio of the polyurethane to the absolute ethyl alcohol to the tetraethoxysilane to the aluminum isopropoxide to the ethyl acetate is 1 g: 30mL of: 0.9 mL: 0.043 g: 1 mL;
(2) placing the prepared porous fiber in a nitric acid solution for light-proof dipping treatment for 18h, filtering, cleaning the porous fiber to be neutral by using deionized water, and drying to obtain pretreated porous fiber;
(3) adding the pretreated porous fiber into an ethanol solution of a silane coupling agent, slowly heating to 60-70 ℃, stirring, refluxing, reacting for 3.5 hours, cooling to room temperature after the reaction is finished, filtering, and drying to obtain the crosslinked porous fiber; wherein the dosage ratio of the pretreated porous fiber to the silane coupling agent is 1 g: 0.04 mL;
(4) dissolving palladium acetate in acetic acid to prepare a palladium acetate solution with the mass concentration of 20%, adding the prepared crosslinked porous fiber, stirring at 30-40 ℃ for 2.5h, adding an ammonia water solution, stirring at normal temperature for reaction for 8h after dropwise addition, filtering, drying, and sintering the dried solid in a muffle furnace at 550-750 ℃ for 4.5h to prepare the porous fiber crosslinking modified hydrogenation catalyst; wherein the mass ratio of the palladium acetate to the cross-linked porous fiber is 1: 5.5;
(5) adding the cracking C10 fraction into a hydrogenation reactor, wherein the hydrogen pressure is 4-8MPa, the hydrogen-oil volume ratio is 500-800, and the volume space velocity is 13-14.5h-1Hydrogenation reaction is carried out at the temperature of 150 ℃ to prepare hydrogenated oil; wherein the mass ratio of the cracking C10 fraction to the catalyst is 20: 0.3;
(6) and adding the prepared hydrogenated oil into a rectifying tower for vacuum rectification, and collecting fractions at the temperature of 165-185 ℃ and 190-220 ℃ to prepare the environment-friendly aromatic hydrocarbon solvent.
The properties of the porous fiber produced according to the present invention and the hydrogenated oil produced were measured, and the results are shown in tables 1 and 2.
TABLE 1
| Diameter, μm | Specific surface area, m2/g | Pore volume, cm3/g | |
| Example 1 | 0.35 | 81.5 | 0.15 |
| Example 2 | 0.30 | 80.3 | 0.13 |
| Example 3 | 0.32 | 81.2 | 0.15 |
| Example 4 | 0.35 | 80.5 | 0.15 |
| Example 5 | 0.33 | 80.9 | 0.18 |
| Example 6 | 0.35 | 81.2 | 0.15 |
TABLE 2
From the test results, the catalyst prepared by the invention has the advantages of sufficient hydrogenation of raw materials, low sulfur content and high yield of environment-friendly solvents.
Although specific embodiments of the invention have been described, many other forms and modifications of the invention will be apparent to those skilled in the art. It is to be understood that the appended claims and this invention generally cover all such obvious forms and modifications which are within the true spirit and scope of the present invention.
Claims (1)
1. The preparation method of the environment-friendly aromatic solvent for the high-grade printing oil is characterized by comprising the following steps of:
(1) dissolving polyurethane in absolute ethyl alcohol to prepare a polyurethane solution; adding tetraethoxysilane, aluminum isopropoxide and ethyl acetate, stirring and mixing, preparing a fiber precursor from the prepared mixed solution by a filamentation process, placing the fiber precursor in a muffle furnace, sintering for 1-4h under inert gas, wherein the sintering temperature is 300-400 ℃, and preparing porous fiber;
(2) placing the prepared porous fiber in a nitric acid solution with the mass concentration of 50-60% for light-proof dipping treatment for 10-20h, filtering, cleaning the porous fiber to be neutral by using deionized water, and drying to obtain the pretreated porous fiber;
(3) adding the pretreated porous fiber into an ethanol solution of a silane coupling agent, slowly heating to 60-70 ℃, stirring, refluxing and reacting for 2-4h, cooling to room temperature after the reaction is finished, filtering, and drying to obtain the crosslinked porous fiber;
(4) dissolving palladium acetate in acetic acid to prepare a palladium acetate solution, wherein the mass concentration of the palladium acetate solution is 15-22%, and then adding the prepared cross-linked porous fiber, wherein the mass ratio of the palladium acetate to the cross-linked porous fiber is 1: (3-6), stirring at 30-40 ℃ for 1-3h, adding an ammonia water solution, after dropwise adding, stirring at normal temperature for reacting for 4-9h, filtering, drying, and sintering the dried solid in a muffle furnace at 550-750 ℃ for 3-5h to obtain the porous fiber crosslinking modified hydrogenation catalyst;
(5) adding the cracked C10 fraction into a hydrogenation reactor filled with a catalyst, wherein the mass ratio of the cracked C10 fraction to the catalyst is (15-22): 0.3, hydrogen pressure is 4-8MPa, hydrogen-oil volume ratio is 500-800, and volume space velocity is 13-14.5h-1Carrying out hydrogenation reaction at the temperature of 130-160 ℃ to obtain hydrogenated oil;
(6) adding the prepared hydrogenated oil into a rectifying tower for vacuum rectification, and collecting fractions at the temperature of 165-185 ℃ and 190-220 ℃ to prepare an environment-friendly aromatic hydrocarbon solvent;
in the step (1), the using amount ratio of the polyurethane to the absolute ethyl alcohol to the ethyl orthosilicate to the aluminum isopropoxide to the ethyl acetate is 1 g: 30mL of: (0.5-1) mL: (0.033-0.045) g: 1 mL; in the step (2), the dosage ratio of the porous fiber to the nitric acid solution is 1 g: (50-60) mL; in the step (3), the dosage ratio of the pretreated porous fiber to the silane coupling agent is 1 g: (0.01-0.05) mL.
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|---|---|---|---|---|
| CN85100760A (en) * | 1985-04-01 | 1986-09-24 | 中国科学院山西煤炭化学研究所 | Hydrofining catalyst for hydrogenation of alkenes and method for making thereof |
| CN103657644A (en) * | 2013-10-31 | 2014-03-26 | 内蒙古工业大学 | Preparation method of novel porous carbon nano fiber loaded palladium nanoparticle composite catalyst |
| CN104152179A (en) * | 2014-09-01 | 2014-11-19 | 江苏联东化工股份有限公司 | Production method of high-boiling-point aromatic solvent oil |
| CN105132019A (en) * | 2015-09-28 | 2015-12-09 | 吴江市万事达环保溶剂有限公司 | Preparation method for high-boiling-point aromatic solvent oil |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100760A (en) * | 1985-04-01 | 1986-09-24 | 中国科学院山西煤炭化学研究所 | Hydrofining catalyst for hydrogenation of alkenes and method for making thereof |
| CN103657644A (en) * | 2013-10-31 | 2014-03-26 | 内蒙古工业大学 | Preparation method of novel porous carbon nano fiber loaded palladium nanoparticle composite catalyst |
| CN104152179A (en) * | 2014-09-01 | 2014-11-19 | 江苏联东化工股份有限公司 | Production method of high-boiling-point aromatic solvent oil |
| CN105132019A (en) * | 2015-09-28 | 2015-12-09 | 吴江市万事达环保溶剂有限公司 | Preparation method for high-boiling-point aromatic solvent oil |
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