CN113896236A - Titanium dioxide synthesis method based on glutamine modification - Google Patents

Titanium dioxide synthesis method based on glutamine modification Download PDF

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CN113896236A
CN113896236A CN202111067439.2A CN202111067439A CN113896236A CN 113896236 A CN113896236 A CN 113896236A CN 202111067439 A CN202111067439 A CN 202111067439A CN 113896236 A CN113896236 A CN 113896236A
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titanium dioxide
glutamine
image analysis
powder
mixed solution
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冒志磊
张丽娜
周军
王淮燕
秦志强
张克良
万婷
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Changzhou Maternal And Child Health Care Hospital
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Changzhou Maternal And Child Health Care Hospital
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Priority to LU500966A priority patent/LU500966B1/en
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Abstract

The invention discloses a method for synthesizing titanium dioxide based on glutamine modification, which belongs to the technical field of biological pharmacy and comprises the following steps: s1, selecting raw materials; s2, preparing a mixed solution A; s3, preparing a mixed solution B; s4, preparing sol; s5, preparing gel; s6, preparation of xerogel powder: drying the wet gel at 100 deg.C for 12 hr, grinding into powder, and calcining the powder at 300 deg.C for 1 hr to remove organic substances; s8, analyzing titanium dioxide. According to the glutamine modification-based titanium dioxide synthesis method, copper ions are doped into nano-particle lattices, lattice stability and lattice energy are reduced, and the copper ions and glutamine react under a neutral condition to obtain glutamine-modified nano-titanium dioxide, so that the glutamine is used for modifying the nano-titanium dioxide, the glutamine-nano-titanium dioxide is synthesized, and ultraviolet, infrared, SEM, EDX and XRD characterization is carried out on the glutamine-modified nano-titanium dioxide for verification.

Description

Titanium dioxide synthesis method based on glutamine modification
Technical Field
The invention belongs to the technical field of biological pharmacy, and particularly relates to a synthesis method of titanium dioxide based on glutamine modification.
Background
Cancer cells have the property of "glutamine addiction" in that they enrich glutamine in large amounts for their rapid growth, and therefore, although glutamine is the most abundant amino acid in the body, a deficiency of glutamine often occurs in tumor-bearing organisms, and thus the supplemented glutamine is rapidly transported to tumor tissues. Although in vitro cell research shows that glutamine can promote tumor cell proliferation, in vivo research results contradict with the results, and the parenteral or enteral nutrition support containing glutamine does not obviously promote tumor growth of tumor-bearing host, probably because glutamine can promote positive nitrogen balance of host and improve body immunity, so that it is safe to supplement glutamine to tumor-bearing body, and the research related to glutamine metabolism is gradually becoming a new target and breakthrough for cancer treatment. The tumor metastasis is inhibited by utilizing the low-toxicity ability but high-efficiency invasion and migration inhibition ability of the nano titanium dioxide, and the nano titanium dioxide is modified by utilizing glutamine, but cannot be directly modified due to large lattice bond energy of the nano titanium dioxide.
In order to solve the above problems, we propose a synthesis method of titanium dioxide based on glutamine modification.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a synthesis method of titanium dioxide based on glutamine modification, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a synthesis method of titanium dioxide based on glutamine modification comprises the following steps:
s1, selecting raw materials: providing a raw material for synthesizing glutamine modified titanium dioxide;
s2, preparing a mixed solution A: selecting butyl titanate, absolute ethyl alcohol and acetylacetone from raw materials, and mixing in a magnetic stirrer to obtain a mixed solution A;
s3, preparing a mixed solution B: selecting anhydrous ethanol and Cu (NO) from raw materials3)2Mixing the aqueous solution and concentrated HCl in a magnetic stirrer to obtain a mixed solution B;
s4, preparing sol: slowly dripping the mixed solution B into the mixed solution A to obtain sol with green color;
s5, preparing gel: putting the prepared sol into a magnetic stirrer, fully and uniformly mixing the sol and the magnetic stirrer, and standing and aging the sol to obtain wet gel;
s6, preparation of xerogel powder: drying the wet gel at 100 ℃ for 12h, grinding the dried gel into powder, roasting the powder at 300 ℃ for 1h to remove organic matters, roasting at 600 ℃ for 2h, and naturally cooling to room temperature to obtain dry gel powder;
s7, modified titanium dioxide: mixing and dissolving the xerogel powder and glutamine in deionized water, adjusting the pH value to 7 by using 0.1mol/L NaOH solution, and reacting for 6 hours to finish the modification of glutamine on titanium dioxide;
s8, analysis of titanium dioxide: and carrying out image analysis on the titanium dioxide modified by the glutamine.
Further optimizing the technical scheme, in S2, the mixing process of the mixed solution a includes the following specific contents: 10ml of butyl titanate was taken and put into a magnetic stirrer, and the butyl titanate was mixed with 8.6ml of absolute ethanol and 0.3ml of acetylacetone under magnetic stirring by the magnetic stirrer.
Further optimizing the technical scheme, in S3, the mixing process of the mixed solution B includes the following specific contents: under magnetic stirring with a magnetic stirrer, 8.6ml of absolute ethanol and 1.3ml of Cu (NO) with a mass concentration of 2%3)2The aqueous solution was mixed well with 0.1ml of concentrated HCl.
Further optimizing the technical scheme, in the step S5, the time for uniformly mixing the sol is 1h, and the temperature for standing and aging the sol is selected from room temperature conditions.
Further optimizing the technical scheme, in the S6, the prepared xerogel powder is modified by Cu2+Ionic titanium dioxide powder.
Further optimizing the technical scheme, in the S7, deionized water used for dissolving xerogel powder and glutamine is heated, and the heating range is 40-50 ℃.
Further optimizing the technical solution, in S8, the image analysis method includes an SEM image analysis method, an XRD image analysis method, an EDX spectrum image analysis method, an ultraviolet spectrum image analysis method, and an infrared spectrum image analysis method.
Further optimizing the technical scheme, when the SEM image analysis method is used for analyzing the glutamine modified titanium dioxide, the microscopic situation of the size, the geometric shape, the uniformity degree and the agglomeration degree of the nano titanium dioxide grains can be visually observed by using a picture shot by a transmission electron microscope.
Further optimizing the technical scheme, when the titanium dioxide modified by glutamine is analyzed by the XRD image analysis method, if the half peak width of the diffraction peak in the XRD pattern of the copper-doped titanium dioxide is widened and the peak position shifts, the copper ions are doped into the titanium dioxide crystal lattice; when the EDX spectral image analysis method is used for analyzing the glutamine modified titanium dioxide, the element content is determined by using an environmental electron scanning microscope with an X-ray energy spectrometer and adopting a selective area quantitative scanning analysis method.
Further optimizing the technical scheme, the ultraviolet spectral image analysis method and the infrared spectral image analysis method perform peak analysis on the ultraviolet visible light absorption spectrum and the infrared visible light absorption spectrum of the titanium dioxide when analyzing the glutamine modified titanium dioxide.
Compared with the prior art, the invention provides a synthesis method of titanium dioxide based on glutamine modification, which has the following beneficial effects:
according to the glutamine modification-based titanium dioxide synthesis method, copper ions are doped into nano-particle lattices, lattice stability and lattice energy are reduced, and the copper ions and glutamine react under a neutral condition to obtain glutamine-modified nano-titanium dioxide, so that the glutamine is used for modifying the nano-titanium dioxide, the glutamine-nano-titanium dioxide is synthesized, and ultraviolet, infrared, SEM, EDX and XRD characterization is carried out on the glutamine-modified nano-titanium dioxide for verification.
Drawings
FIG. 1 is a schematic flow chart of a method for synthesizing titanium dioxide based on glutamine modification according to the present invention;
FIG. 2 is a surface appearance picture of a nano titanium dioxide sample modified with copper ions observed by an SEM image analysis method in a titanium dioxide synthesis method based on glutamine modification according to the present invention;
FIG. 3 is a surface appearance picture of a glutamine-modified nano titanium dioxide sample observed by an SEM image analysis method in a glutamine-modified titanium dioxide synthesis method provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
The first embodiment is as follows:
referring to fig. 1, a method for synthesizing titanium dioxide based on glutamine modification includes the following steps:
s1, selecting raw materials: providing a raw material for synthesizing glutamine modified titanium dioxide;
s2, preparing a mixed solution A: selecting butyl titanate, absolute ethyl alcohol and acetylacetone from raw materials, and mixing in a magnetic stirrer to obtain a mixed solution A;
s3, preparing a mixed solution B: selecting anhydrous ethanol and Cu (NO) from raw materials3)2Mixing the aqueous solution and concentrated HCl in a magnetic stirrer to obtain a mixed solution B;
s4, preparing sol: slowly dripping the mixed solution B into the mixed solution A to obtain sol with green color;
s5, preparing gel: putting the prepared sol into a magnetic stirrer, fully and uniformly mixing the sol and the magnetic stirrer, and standing and aging the sol to obtain wet gel;
s6, preparation of xerogel powder: drying the wet gel at 100 ℃ for 12h, grinding the dried gel into powder, roasting the powder at 300 ℃ for 1h to remove organic matters, roasting at 600 ℃ for 2h, and naturally cooling to room temperature to obtain dry gel powder;
s7, modified titanium dioxide: mixing and dissolving the xerogel powder and glutamine in deionized water, adjusting the pH value to 7 by using 0.1mol/L NaOH solution, and reacting for 6 hours to finish the modification of glutamine on titanium dioxide;
s8, analysis of titanium dioxide: and carrying out image analysis on the titanium dioxide modified by the glutamine.
Specifically, in S2, the mixing process of the mixed solution a includes the following specific contents: 10ml of butyl titanate was taken and put into a magnetic stirrer, and the butyl titanate was mixed with 8.6ml of absolute ethanol and 0.3ml of acetylacetone under magnetic stirring by the magnetic stirrer.
Specifically, in S3, the mixing process of the mixed solution B includes the following specific contents: under magnetic stirring with a magnetic stirrer, 8.6ml of absolute ethanol and 1.3ml of Cu (NO) with a mass concentration of 2%3)2The aqueous solution was mixed well with 0.1ml of concentrated HCl.
Specifically, in the step S5, the time for uniformly mixing the sol is 1 hour, and the temperature for standing and aging the sol is selected from room temperature conditions.
Specifically, in the S6, the prepared xerogel powder is modified by Cu2+Ionic titanium dioxide powder.
Specifically, in the S7, deionized water for dissolving xerogel powder and glutamine is heated, and the heating range is 40-50 ℃.
Specifically, in S8, the image analysis method includes SEM image analysis, XRD image analysis, EDX spectrum image analysis, ultraviolet spectrum image analysis, and infrared spectrum image analysis.
Specifically, when the SEM image analysis method is used for analyzing the glutamine modified titanium dioxide, the microscopic conditions of the size, the geometric shape, the uniformity degree and the agglomeration degree of the nano titanium dioxide crystal grains can be visually observed by using a picture shot by a transmission electron microscope.
Specifically, when the glutamine modified titanium dioxide is analyzed by the XRD image analysis method, if the half width of a diffraction peak in an XRD pattern of the copper-doped titanium dioxide is widened and the peak position is shifted, copper ions are doped into a titanium dioxide crystal lattice; when the EDX spectral image analysis method is used for analyzing the glutamine modified titanium dioxide, the element content is determined by using an environmental electron scanning microscope with an X-ray energy spectrometer and adopting a selective area quantitative scanning analysis method.
Specifically, the ultraviolet spectral image analysis method and the infrared spectral image analysis method perform peak analysis on the ultraviolet visible light absorption spectrum and the infrared visible light absorption spectrum of titanium dioxide when analyzing the glutamine modified titanium dioxide.
Example two:
the synthesized titanium dioxide was analyzed by SEM image analysis, XRD image analysis, EDX spectral image analysis, ultraviolet spectral image analysis, and infrared spectral image analysis using the method for synthesizing titanium dioxide based on glutamine modification described in example one.
SEM image analysis method: as shown in fig. 2, microscopic conditions such as the size, the geometric shape, the uniformity, the agglomeration degree and the like of the copper ion modified nano titanium dioxide crystal grains can be visually observed by using a photograph taken by a transmission electron microscope, and the sample crystal grains are irregular rectangles and have good dispersibility. As shown in fig. 3, the SEM result of the glutamine modified product showed that the morphology was changed from that of fig. 2, most of the particles were cubic, and the surface of the cube was loaded with fine spherical particles, which resulted in partial agglomeration.
XRD spectral image analysis method: the particle sizes of the titanium dioxide and the Cu/titanium dioxide are calculated according to a Sherrer formula and are respectively 29nm and 24-25 nm. As can be seen from the XRD pattern of the copper-doped titanium dioxide and the XRD pattern of the pure titanium dioxide, the half width of the diffraction peak in the XRD pattern of the copper-doped titanium dioxide becomes wider and the peak positions shift, indicating that copper ions have been incorporated into the titanium dioxide crystal lattice.
EDX spectral image analysis method: the element content determination is accomplished by using an environmental electron scanning microscope with an X-ray spectrometer and using a selected area quantitative scanning analysis method.
Ultraviolet spectrum image analysis method and infrared spectrum image analysis method: the copper-doped titanium dioxide sample has a wide absorption band of 400-800 nm. At 3425cm-1Near infrared absorption corresponds to H-N and O-H stretching vibrations, 1705cm-1The absorption peak at (a) is attributed to the stretching vibration of the C ═ O bond. The absorption vibration peak value of the copper-doped titanium dioxide is 500-520 cm-1The vibration peak in this interval is the Ti-O bond vibration peak. The sample of the purified composite particles is 3425cm and 1705cm-1And obvious characteristic absorption bands of glutamine exist at the positions, which fully indicates that partial glutamine molecules are modified on the surface of the Cu/titanium dioxide nano particle.
The invention has the beneficial effects that: according to the glutamine modification-based titanium dioxide synthesis method, copper ions are doped into nano-particle lattices, lattice stability and lattice energy are reduced, and the copper ions and glutamine react under a neutral condition to obtain glutamine-modified nano-titanium dioxide, so that the glutamine is used for modifying the nano-titanium dioxide, the glutamine-nano-titanium dioxide is synthesized, and ultraviolet, infrared, SEM, EDX and XRD characterization is carried out on the glutamine-modified nano-titanium dioxide for verification.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. A synthesis method of titanium dioxide based on glutamine modification is characterized by comprising the following steps:
s1, selecting raw materials: providing a raw material for synthesizing glutamine modified titanium dioxide;
s2, preparing a mixed solution A: selecting butyl titanate, absolute ethyl alcohol and acetylacetone from raw materials, and mixing in a magnetic stirrer to obtain a mixed solution A;
s3, preparing a mixed solution B: selecting anhydrous ethanol, a Cu (NO3)2 aqueous solution and concentrated HCl from raw materials, and mixing in a magnetic stirrer to obtain a mixed solution B;
s4, preparing sol: slowly dripping the mixed solution B into the mixed solution A to obtain sol with green color;
s5, preparing gel: putting the prepared sol into a magnetic stirrer, fully and uniformly mixing the sol and the magnetic stirrer, and standing and aging the sol to obtain wet gel;
s6, preparation of xerogel powder: drying the wet gel at 100 ℃ for 12h, grinding the dried gel into powder, roasting the powder at 300 ℃ for 1h to remove organic matters, roasting at 600 ℃ for 2h, and naturally cooling to room temperature to obtain dry gel powder;
s7, modified titanium dioxide: mixing and dissolving the xerogel powder and glutamine in deionized water, adjusting the pH value to 7 by using 0.1mol/L NaOH solution, and reacting for 6 hours to finish the modification of glutamine on titanium dioxide;
s8, analysis of titanium dioxide: and carrying out image analysis on the titanium dioxide modified by the glutamine.
2. The method for synthesizing titanium dioxide based on glutamine modification according to claim 1, wherein in the step S2, the mixing process of the mixed solution A comprises the following specific contents: 10ml of butyl titanate was taken and put into a magnetic stirrer, and the butyl titanate was mixed with 8.6ml of absolute ethanol and 0.3ml of acetylacetone under magnetic stirring by the magnetic stirrer.
3. The method for synthesizing titanium dioxide based on glutamine modification according to claim 1, wherein in the step S3, the mixing process of the mixed solution B comprises the following specific steps: under magnetic stirring with a magnetic stirrer, 8.6ml of absolute ethyl alcohol and 1.3ml of Cu (NO3) with a mass concentration of 2%2The aqueous solution was mixed well with 0.1ml of concentrated HCl.
4. The method for synthesizing titanium dioxide based on glutamine modification according to claim 1, wherein in S5, the time for mixing the sol is 1h, and the temperature for standing and aging the sol is selected as the room temperature condition.
5. The method for synthesizing titanium dioxide based on glutamine modification according to claim 1, wherein in S6, the dry gel powder is Cu modified2+Ionic titanium dioxide powder.
6. The method for synthesizing titanium dioxide based on glutamine modification according to claim 1, wherein in the S7, deionized water for dissolving xerogel powder and glutamine is heated, and the heating range is 40-50 ℃.
7. The glutamine modification-based titanium dioxide synthesis method according to claim 1, wherein in the step S8, the image analysis method includes SEM image analysis, XRD image analysis, EDX spectrum image analysis, ultraviolet spectrum image analysis, and infrared spectrum image analysis.
8. The method for synthesizing titanium dioxide based on glutamine modification according to claim 7, wherein when analyzing the glutamine modified titanium dioxide, the SEM image analysis method is used for visually observing the microscopic conditions of the size, the geometric shape, the uniformity degree and the agglomeration degree of the nano titanium dioxide crystal grains by using a photo taken by a transmission electron microscope.
9. The glutamine modified titanium dioxide synthesis method according to claim 7, characterized in that, when the glutamine modified titanium dioxide is analyzed by the XRD image analysis method, if the half width of the diffraction peak in the XRD pattern of the copper-doped titanium dioxide is widened and the peak position is shifted, the copper ions are doped into the titanium dioxide crystal lattice; when the EDX spectral image analysis method is used for analyzing the glutamine modified titanium dioxide, the element content is determined by using an environmental electron scanning microscope with an X-ray energy spectrometer and adopting a selective area quantitative scanning analysis method.
10. The method for synthesizing titanium dioxide based on glutamine modification according to claim 7, wherein the ultraviolet spectral image analysis method and the infrared spectral image analysis method perform peak analysis on the ultraviolet visible light absorption spectrum and the infrared visible light absorption spectrum of titanium dioxide when analyzing the glutamine modified titanium dioxide.
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