CN111393661A - Large-scale room temperature preparation method of heterogeneous demulsifier MI L-100 (Fe) crystal material - Google Patents
Large-scale room temperature preparation method of heterogeneous demulsifier MI L-100 (Fe) crystal material Download PDFInfo
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Abstract
The invention provides a large-scale room temperature preparation method of a heterogeneous demulsifier MI L-100 (Fe) crystal material, which is based on a thermodynamic spontaneous reaction and molecular self-assembly method and utilizes Fe by controlling a reaction path3+The method has the advantages of simple operation and low cost, does not need to provide extra energy required by heating, does not need to provide a special reactor required by high-temperature and high-pressure/microwave synthesis/mechanical synthesis/electrochemical reaction, and does not need to add other toxic and harmful reagents such as acid, alkali, coordination regulator and the likeThe post-modification can realize excellent demulsification performance, and can be used as an efficient non-load type heterogeneous demulsifier for application in the fields of petrochemical industry, environmental pollution remediation and the like.
Description
Technical Field
The invention relates to the technical field of metal organic framework material preparation, in particular to a preparation method of an unsupported heterogeneous demulsifier for efficient demulsification in the fields of petrochemical industry, environmental pollution remediation and the like.
Background
The high water content of petroleum produced fluids is extremely detrimental to subsequent transportation, refining, etc. of the petroleum produced fluids, which can cause significant economic loss due to corrosion of pipelines and equipment, thus, dehydration of crude oil emulsions with high water content is one of the major research fields of the current petrochemical industry, furthermore, oil spill, oil-containing wastewater discharge of the petrochemical industry, wastewater discharge of life, metallurgy, traffic, etc. lead to increasingly severe oil contamination of water bodies, which increases environmental burden, demulsification of oil phases in water bodies can form stable emulsions under the emulsification action of surfactants, which increases the difficulty in remediation of water environmental pollution, whether dehydration of crude oil or remediation of oil-containing pollution, which is one of the key technologies of demulsification, and remediation of water environmental pollution, which is based on the fact that the demulsifiers have high energy and chemical flooding, which are the most important factors of conventional demulsification and the demulsification water phase and salinity are generally required to achieve the same order of magnitude of water phase and salinity of water pollution, which are generally required to achieve the same magnitude of water phase and salinity of demulsification, which are generally required to achieve the same magnitude of water phase-water pollution.
The metal organic framework material is a potential non-load type intrinsic demulsification material, however, no relevant clear report exists at present, aiming at a typical metal organic framework material MI L-100 (Fe), the preparation method of the metal organic framework material generally needs to be carried out at high temperature and high pressure, so that the large-scale preparation and application of the metal organic framework material are restricted, and HF/HNO needs to be added3NaOH and other acid-base regulators or N, N-dimethylformamide/triethylamine and other organic solvents do not accord with the economic, green and environment-friendly material preparation idea.
In addition, MI L-100 (Fe) is widely used for drug loading and diagnosis research as an MOFs material with high biological safety, however, bioactive molecules can not keep activity under extreme conditions such as acid/alkali, high temperature/high pressure, and the like, so that the traditional MI L-100 (Fe) synthesis method can not well meet the research requirements of the life field, and thus, a method for preparing the MI L-100 (Fe) crystal material under the conditions of low temperature and normal pressure and avoiding using various regulators is urgently required to ensure that the MI L-100 (Fe) crystal material with rich pores is prepared under the condition as mild as possible, and therefore, the invention provides a large-scale preparation method of the MI L-100 (Fe) crystal material at room temperature.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provide a method for preparing the MI L-100 (Fe) crystal material with high porosity simply, with low energy consumption, environmental protection, safety and rapidness at room temperature, and the method can be used for large-scale preparation.
The invention aims to provide the demulsification application of the MI L-100 (Fe) crystal material as a high-efficiency non-load heterogeneous demulsifier in the fields of petrochemical industry, environmental pollution remediation and the like.
The invention aims to realize the purpose of the invention by adopting the following technical scheme that the large-scale room temperature preparation method of the crystalline material of the heterogeneous demulsifier MI L-100 (Fe) comprises the following steps:
(1) preparing Fe with a certain concentration3+Aqueous and methanol solutions of trimesic acid;
(2) dropwise adding methanol solution of trimesic acid to Fe in a stirring state at room temperature3+Adding the solution into the solution, and continuously stirring the solution for a period of time to obtain an unloaded MI L-100 (Fe) heterogeneous demulsifier crystal material;
(3) the prepared MI L-100 (Fe) crystal material powder is put into the emulsion in a certain mode, and the emulsion breaking can be realized efficiently by shaking for a certain time.
Further, a method for preparing MI L-100 (Fe) crystal material in large scale at room temperature and application of the MI L-100 (Fe) crystal material as high-efficiency non-load heterogeneous demulsifier are described above, and in the step (1), the Fe is used3+Solutions include, but are not limited to, inorganic Fe such as ferric trichloride solutions, ferric nitrate solutions, and ferric sulfate solutions3+A salt solution.
Further, the large-scale room temperature preparation method of the heterogeneous demulsifier MI L-100 (Fe) crystal material comprises the step (1) of preparing the trimesic acid and Fe3+The molar ratio of (A) to (B) is 1: 3-3: 1.
Further, in the large-scale room temperature preparation method of the crystalline material of the heterogeneous demulsifier MI L-100 (Fe) as described above, in the step (2), the dripping rate of the methanol solution of the trimesic acid is not more than 5 drops/second.
Further, a large scale room temperature preparation method of the crystalline material of the heterogeneous demulsifier MI L-100 (Fe) as described above, step (2), under room temperature conditions, does not require heating.
Further, in the large-scale room temperature preparation method of the crystalline material of the heterogeneous demulsifier MI L-100 (Fe) as described above, in the step (2), the methanol solution of the trimesic acid is required to be added dropwise to the Fe under the stirring state3+In aqueous solution.
Further, a large-scale room temperature preparation method of the crystalline material of the heterogeneous demulsifier MI L-100 (Fe) as described above, in step (2), the stirring time is continued for not less than 2 hours.
Further, the large-scale room temperature preparation method of the heterogeneous demulsifier MI L-100 (Fe) crystalline material, as described above, in step (3), the adding manner of the prepared MI L-100 (Fe) crystalline material powder includes, but is not limited to, a direct powder adding manner and a suspension adding manner of preparing the powder.
Further, the large-scale room temperature preparation method of the heterogeneous demulsifier MI L-100 (Fe) crystalline material, as described above, in the step (3), the demulsification application of the MI L-100 (Fe) crystalline material is to be carried out by using an emulsion prepared by an anionic surfactant or a nonionic surfactant, and a crude oil emulsion.
Compared with the traditional MI L-100 (Fe) crystal material preparation method, the method has the advantages of simple operation, low cost, no need of additional toxic and harmful reagents such as acid and alkali, organic reagents and the like, and no limitation of synthesis places/containers, and meanwhile, the synthesized MI L-100 (Fe) crystal material has the characteristics of large specific surface area and high porosity, and the prepared MI L-100 (Fe) crystal material has excellent demulsification performance, so the method has important application value in the fields of petrochemical industry, environmental pollution remediation and the like.
Drawings
FIG. 1 is a pictorial representation of a crystalline MI L-100 (Fe) material prepared in accordance with an embodiment of the present invention;
FIG. 2 is an X-ray diffraction pattern of a crystalline MI L-100 (Fe) material prepared by an example of the present invention;
FIG. 3 is a plot of the pore size distribution of MI L-100 (Fe) crystalline material prepared in accordance with an embodiment of the present invention;
FIG. 4 is a N of MI L-100 (Fe) crystals prepared by an example of the present invention2Isothermal adsorption/desorption curves;
FIG. 5 is a scanning electron micrograph of MI L-100 (Fe) crystalline material prepared according to an example of the present invention;
FIG. 6 is a graph of the demulsifying effect of MI L-100 (Fe) crystalline material on anionic surfactant model emulsions prepared in accordance with an embodiment of the present invention
FIG. 7 is a graph of the demulsifying effect of MI L-100 (Fe) crystalline material prepared in accordance with an embodiment of the present invention on a crude oil emulsion having a water content of 10%;
FIG. 8 is a bar graph of the demulsification efficiency of MI L-100 (Fe) crystalline material made by an example of the present invention against the pH effects of an anionic surfactant model emulsion;
FIG. 9 is a bar graph of demulsification efficiency of MI L-100 (Fe) crystalline material made by an example of the present invention with respect to salinity effects of anionic surfactant model emulsions;
FIG. 10 is a bar graph of the demulsification efficiency of MI L-100 (Fe) crystalline materials prepared according to an example of the present invention for different types of model emulsions.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention are described below clearly and completely, and it is obvious that the described embodiments are some, not all embodiments of the present invention. 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.
Example (b):
(1) 120g of FeCl is taken3·6H2Dissolving O in 500ml water to prepare Fe3+Dissolving 42g of trimesic acid in 800ml of methanol to prepare a methanol solution of trimesic acid;
(2) 800ml of the above-mentioned methanol solution of trimesic acid was added dropwise to Fe under stirring at room temperature3+Solutions ofAnd then centrifuging, washing, drying and grinding to obtain an orange powdery sample, namely the MI L-100 (Fe) crystal material.
Application example 1
Demulsification of model emulsions by MI L-100 (Fe) crystalline materials:
preparation of anionic surfactant model emulsion: taking 200ml of water, adding 0.2g of sodium dodecyl sulfate to completely dissolve the water, adding 40ml of oleic acid, and shearing the mixture for 90 seconds at the rotating speed of 3800 rpm by using a homogenizing stirrer to prepare the anionic surfactant model emulsion.
0.20g of the prepared crystalline material MI L-100 (Fe) was taken, 19.6ml of water was added, and then 0.4ml of anionic surfactant model emulsion was added.
And (3) manually oscillating the system for 15 seconds, standing for 5 minutes, repeating the oscillation-standing operation for multiple times within 30 minutes to realize demulsification, measuring the absorbance of the system before and after demulsification by using an ultraviolet-visible spectrophotometer, and calculating the demulsification rate of the MI L-100 (Fe) crystal material on the model emulsion.
Application example 2
Demulsification stability test of MI L-100 (Fe) crystalline material against pH influence
0.10g of the prepared crystalline MI L-100 (Fe) material was placed in a number of clear glass bottles, followed by addition of 19.6ml of each of water at pH 2.0, 4.0, 6.0, 8.0 and 10.0, followed by the addition of 0.4ml of anionic surfactant model emulsion.
And (3) manually oscillating the system for 15 seconds, standing for 5 minutes, repeating the oscillation-standing operation for multiple times within 30 minutes to realize demulsification, measuring the absorbance of the system before and after demulsification by using an ultraviolet-visible spectrophotometer, and calculating the demulsification rate of the MI L-100 (Fe) crystal material on the model emulsion.
Application example 3
Demulsification stability test for resisting salinity influence of MI L-100 (Fe) crystalline material
0.10g of the prepared crystalline MI L-100 (Fe) material was placed in a number of clear glass bottles, followed by addition of 19.6ml of aqueous sodium chloride solutions of 1, 10, 100 and 1000 mmol/L each, followed by the addition of 0.4ml of anionic surfactant model emulsion in that order.
And (3) manually oscillating the system for 15 seconds, standing for 5 minutes, repeating the oscillation-standing operation for multiple times within 30 minutes to realize demulsification, measuring the absorbance of the system before and after demulsification by using an ultraviolet-visible spectrophotometer, and calculating the demulsification rate of the MI L-100 (Fe) crystal material on the model emulsion.
Application example 4
Demulsification of MI L-100 (Fe) crystalline materials to different kinds of model emulsions:
preparation of nonionic surfactant model emulsion: 200ml of water is taken, 1.0g of Tween-80 is added to be completely dissolved, 40ml of oleic acid is added, and the mixture is sheared for 90 seconds at the rotating speed of 3800 revolutions per minute by a homogenizing stirrer to prepare the nonionic surfactant model emulsion.
0.10g of the prepared MI L-100 (Fe) crystalline material was put in a plurality of transparent glass bottles, 19.6ml of water was added, and 0.4ml of an anionic surfactant model emulsion and a nonionic surfactant model emulsion were sequentially added.
And (3) manually oscillating the system for 15 seconds, standing for 5 minutes, repeating the oscillation-standing operation for multiple times within 30 minutes to realize demulsification, measuring the absorbance of the system before and after demulsification by using an ultraviolet-visible spectrophotometer, and calculating the demulsification rate of the MI L-100 (Fe) crystal material on the model emulsion.
Application example 5
Crude oil emulsion dehydration of MI L-100 (Fe) crystalline material:
preparation of crude oil emulsion: adding 2ml of crude oil into 18ml of water, and violently shaking for a certain time to prepare a crude oil emulsion with the water content of 90%; the crude oil emulsion does not have oil-water separation phenomenon within 2 hours in water bath at 60 ℃.
0.10g of prepared MI L-100 (Fe) crystal material is added into the freshly prepared crude oil emulsion, the crude oil emulsion with high water content is dehydrated after manual shaking for 10 seconds and standing for 5 minutes, and the dehydration rate of the MI L-100 (Fe) crystal material to the crude oil emulsion is calculated by measuring the volume of the aqueous solution after the crude oil emulsion is dehydrated.
FIG. 1 is a diagram of a sample prepared in example, and it can be seen that the sample prepared in example is orange powder.
FIG. 2 is an X-ray diffraction pattern of the sample prepared in example 1, showing that characteristic diffraction peaks of MI L-100 (Fe) crystals appear at 5.07 deg., 10.32 deg., 10.95 deg., etc., and in the range of 12 deg. to 30 deg., indicating that the sample prepared in example has a crystal structure of MI L-100 (Fe), and thus the sample prepared in example is a pure MI L-100 (Fe) crystal material.
FIG. 3 is a scanning electron microscope image of MI L-100 (Fe) crystalline material prepared according to an example of the present invention, showing that the MI L-100 (Fe) crystalline material has a particle size of about 300 nm.
FIG. 4 shows N of MI L-100 (Fe) crystalline material prepared in example2The isothermal adsorption/desorption curves show the N of the MI L-100 (Fe) crystalline material2The isothermal adsorption/desorption curve corresponds to the type i curve of the IUPAC classification.
FIG. 5 is a plot of the pore size distribution of the crystalline MI L-100 (Fe) material prepared in the examples, showing that the MI L-100 (Fe) material has pore sizes of 1.1, 2.0 and 2.5nm, and the BET specific surface area of the crystalline MI L-100 (Fe) material prepared in the examples is calculated to be 1344m2Per g, pore volume 0.727cm3The MI L-100 (Fe) crystalline material prepared in the examples had a rich pore structure.
FIG. 6 is a graph showing the demulsification effect of MI L-100 (Fe) crystalline materials on anionic surfactant model emulsions and crude oil emulsions having a water content of 10% prepared in example of the present invention, wherein the anionic surfactant model emulsions were demulsified with MI L-100 (Fe) crystalline materials under the conditions of application example 1 described above, the liquids were colorless and transparent, and the demulsification rate was better than 99%.
FIG. 7 is a graph showing the demulsification effect of MI L-100 (Fe) crystalline materials prepared in the example of the present invention on crude oil emulsions having a water content of 10%, under the conditions of application example 5, the crude oil emulsions were demulsified by MI L-100 (Fe) crystalline materials, and the dehydrated oil phase and water phase interface was clear, and the dehydration rate of the crude oil emulsion was better than 75% in 5 minutes.
FIG. 8 is a bar graph of the demulsification efficiency of MI L-100 (Fe) crystalline materials prepared by the embodiment of the invention on the pH influence of an anionic surfactant model emulsion, wherein the demulsification efficiency of the MI L-100 (Fe) crystalline materials on the model emulsion is not reduced in the pH range of 4.0-10.0, which shows that the demulsification performance of the MI L-100 (Fe) crystalline materials has stable demulsification performance in the pH range of 4.0-10.0, the demulsification efficiency of the MI L-100 (Fe) crystalline materials is increased in the pH range of 2.0, and the MI L-100 (Fe) crystalline materials are more suitable for demulsification under acidic conditions.
FIG. 9 is a bar graph of the demulsification efficiency of MI L-100 (Fe) crystalline material against the effects of salinity on anionic surfactant model emulsions prepared according to examples of the present invention, showing that the demulsification efficiency of MI L-100 (Fe) crystalline material on model emulsions gradually increases as the concentration of NaCl increases from 0 to 1000 mmol/L, indicating that salinity does not adversely affect the demulsification performance of MI L-100 (Fe) crystalline material.
FIG. 10 is a bar graph showing the demulsification efficiency of MI L-100 (Fe) crystalline materials prepared in the example of the present invention against different types of model emulsions, wherein the demulsification rates of MI L-100 (Fe) crystalline materials against anionic surfactant model emulsions and nonionic surfactant model emulsions are 94% and 91%, respectively, under the conditions of the application example 4, which shows that MI L-100 (Fe) crystalline materials have good demulsification effects against both anionic surfactant emulsions and nonionic surfactant emulsions.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A large-scale room temperature preparation method of a heterogeneous demulsifier MI L-100 (Fe) crystal material is characterized by comprising the following steps:
(1) configuration ofA certain concentration of Fe3+Aqueous and methanol solutions of trimesic acid;
(2) dropwise adding methanol solution of trimesic acid to Fe in a stirring state at room temperature3+Adding into the solution, and stirring for a while to obtain MI L-100 (Fe) crystal material;
(3) the prepared MI L-100 (Fe) crystal material powder is put into the emulsion in a certain mode, and the emulsion breaking can be realized efficiently by shaking for a certain time.
2. The large-scale room temperature preparation method of the crystalline material of the heterogeneous demulsifier MI L-100 (Fe) according to claim 1, wherein in step (1), the Fe is3+Aqueous solutions include, but are not limited to FeCl3、Fe(NO3)3And Fe2(SO4)3And aqueous solutions of the corresponding hydrates, and the like.
3. The large-scale room temperature preparation method of a heterogeneous demulsifier MI L-100 (Fe) crystal material of claim 1, wherein in step (1), the Fe is3+The mol ratio of the trimesic acid to the trimesic acid is 1: 3-3: 1.
4. The large-scale room temperature preparation method of the crystalline material of the heterogeneous demulsifier MI L-100 (Fe) according to claim 1, wherein in the step (2), the dropwise addition rate of the trimesic acid is not more than 5 drops/s.
5. The large-scale room temperature preparation method of the crystalline material of the heterogeneous demulsifier MI L-100 (Fe) according to claim 1, wherein in the step (2), the methanol solution of trimesic acid is added dropwise at room temperature, and the room temperature is not critical.
6. The large-scale room temperature preparation method of the crystalline material of the heterogeneous demulsifier MI L-100 (Fe) according to claim 1, wherein in the step (2), the methanol solution of trimesic acid is added dropwise to Fe under stirring3+In aqueous solution, stirring speedThe degree is preferably but not strictly limited to the occurrence of vortices.
7. The large-scale room temperature preparation method of the crystalline material of the heterogeneous demulsifier MI L-100 (Fe) according to claim 1, wherein the continuous stirring time in step (2) is not less than 2 hours.
8. The large-scale room temperature preparation method of the crystalline material of the heterogeneous demulsifier MI L-100 (Fe) according to claim 1, wherein in the step (3), the MI L-100 (Fe) crystalline material powder is added in a manner including, but not limited to, a direct powder adding manner and a suspension adding manner.
9. The method for preparing the heterogeneous demulsifier MI L-100 (Fe) crystalline material at room temperature on a large scale according to claim 1, wherein in step (3), the MI L-100 (Fe) crystalline material demulsification application object emulsion comprises but is not limited to anionic surfactant emulsion and nonionic surfactant emulsion, and crude oil emulsion.
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