Method and equipment for synthesizing ultraviolet light absorber

Abstract

The invention discloses an ultraviolet light absorber synthesis method and equipment, and the synthesis method comprises the following steps: S1, dissolving an alcohol-soluble monascus pigment in a mixed solvent of absolute methanol and ethanol, and adding 5% of a Pd / C catalyst; s2, under the protection of nitrogen, carrying out magnetic stirring reaction for 8 hours; s3, filtering to remove the catalyst, concentrating the reaction liquid, purifying by silica gel column chromatography, eluting with ethyl acetate / petroleum ether, concentrating and drying; s4, dissolving the monascus pigment derivative, an organic ultraviolet light absorber and a light stabilizer in an organic solvent; s5, adding a nano material, and performing ultrasonic dispersion for 20 minutes; s6, adding polyurethane and amino polysiloxane microemulsion, and stirring for 1 hour to obtain a homogeneous solution; s7, the homogeneous solution is put into purification equipment for purification and impurity removal treatment, and finally the ultraviolet light absorber is obtained. According to the preparation method of the ultraviolet light absorber, through the synergistic effect of the monascus pigment derivative and the organic ultraviolet light absorber, the UVA and UVB full wave band 200-400 nm is covered; the water washing resistance is good; the environment-friendly effect is good.

Description

Technical Field

[0001] The present invention relates to the technical field of synthetic methods of ultraviolet absorbers, and particularly relates to a synthetic method and equipment for ultraviolet absorbers. Background Art

[0002] In the prior art, ultraviolet absorbers mainly include two categories: inorganic type and organic type. Inorganic ultraviolet absorbers (such as nano-TiO2, ZnO) have problems such as poor dispersibility and affecting the hand feeling of fabrics; although organic ultraviolet absorbers (such as benzotriazoles, triazines) have good absorption effects, they have poor wash resistance, and some components have the risk of biological toxicity.

[0003] When the existing ultraviolet absorbers are used alone, their wash resistance and stability are insufficient; moreover, the ultraviolet absorbers relying on traditional chemical synthesis are insufficient in environmental protection. Summary of the Invention

[0004] The problems to be solved by the present invention are: to provide a synthetic method and equipment for ultraviolet absorbers, which, through the synergistic effect of monascus pigment derivatives and organic ultraviolet absorbers, cover the entire UVA and UVB bands of 200-400 nm; polyurethane and nanomaterials form a network structure, significantly improving the adhesion and having good wash resistance; monascus pigment derivatives replace part of the synthetic ultraviolet absorbers, reducing the ecological risk; the catalytic hydrogenation conditions are mild, and chromatographic purification accurately enriches the effective components.

[0005] The technical solution provided by the present invention to solve the above problems is: a synthetic method of an ultraviolet absorber, the ultraviolet absorber comprises the following components by weight: 10-30 parts of monascus pigment derivatives, 5-15 parts of organic ultraviolet absorbers, 5-20 parts of polyurethane, 1-5 parts of nanomaterials, 1-3 parts of light stabilizers, and 30-60 parts of solvents.

[0006] Preferably, the ultraviolet absorber comprises the following components by weight: 10 parts of monascus pigment derivatives, 7 parts of organic ultraviolet absorbers, 8 parts of polyurethane, 1 part of nanomaterials, 1 part of light stabilizers, and 30 parts of solvents.

[0007] Preferably, the ultraviolet absorber comprises the following components by weight: 20 parts of monascus pigment derivatives, 5 parts of organic ultraviolet absorbers, 15 parts of polyurethane, 3 parts of nanomaterials, 2 parts of light stabilizers, and 40 parts of solvents.

[0008] Preferably, the ultraviolet absorber comprises the following components by weight: 30 parts of monascus pigment derivatives, 15 parts of organic ultraviolet absorbers, 18 parts of polyurethane, 5 parts of nanomaterials, 3 parts of light stabilizers, and 50 parts of solvents.

[0009] Preferably, the synthetic method comprises the following steps

[0010] S1. Dissolve the alcohol-soluble monascus pigment in a mixed solvent of absolute methanol and ethanol with a volume ratio of 1:1, and add 5% Pd / C catalyst.

[0011] S2. Under nitrogen protection, magnetically stir and react at 40 °C and 0.3 MPa for 8 h.

[0012] S3. Filter to remove the catalyst, concentrate the reaction solution, purify it by silica gel column chromatography, elute with ethyl acetate / petroleum ether, collect the components with ultraviolet absorption peaks at 280 - 350 nm, and concentrate and dry.

[0013] S4. Dissolve the monascus pigment derivative, organic ultraviolet absorber, and light stabilizer in an organic solvent.

[0014] S5. Add the nanomaterial and ultrasonically disperse for 20 min.

[0015] S6. Add polyurethane and amino polysiloxane microemulsion and stir for 1 h to obtain a homogeneous solution.

[0016] S7. Put the homogeneous solution into a purification device for purification and impurity removal treatment, and finally obtain the ultraviolet absorber.

[0017] Preferably, the dosage of the Pd / C catalyst in S1 is 10 wt% of the raw materials.

[0018] Preferably, the organic solvent in S4 is a mixture of ethanol and ethyl acetate with a volume ratio of 3:1.

[0019] Preferably, the nanomaterial in S5 is nanometer TiO2 modified by a silane coupling agent with a particle size of 20 - 50 nm.

[0020] Preferably, the polyurethane in S6 is an anionic aqueous polyurethane with a molecular weight of 5000 - 10000.

[0021] Preferably, the purification device in S7 includes a purification barrel; a filter assembly is arranged in the purification barrel; the filter assembly includes a plurality of filter columns; each filter column includes a fixed outer shell and a hollow fiber membrane tube, the hollow fiber membrane tube is arranged in the fixed outer shell, and a through hole for liquid to flow through is arranged on the fixed outer shell; a purification chamber and a collection chamber are arranged in the purification barrel, the purification chamber is arranged above the collection chamber, a plurality of purification holes are arranged in the purification chamber, the filter columns are detachably installed in the purification holes, and the inner cavity of the hollow fiber membrane tube is communicated with the collection chamber.

[0022] Compared with the prior art, the advantages of the present invention are as follows: The preparation method of the ultraviolet absorber of the present invention synergistically uses monascus pigment derivatives and organic ultraviolet absorbers to cover the entire UVA and UVB bands of 200-400 nm; polyurethane and nanomaterials form a network structure, significantly improving the adhesion and having good wash resistance; monascus pigment derivatives replace part of the synthetic ultraviolet absorber, reducing the ecological risk; the catalytic hydrogenation conditions are mild, and chromatographic purification accurately enriches the active ingredients. Description of the Drawings

[0023] The drawings described herein are used to provide a further understanding of the present invention, and constitute a part of the present invention. The schematic embodiments and descriptions thereof of the present invention are used to explain the present invention and do not constitute an improper limitation of the present invention.

[0024] Figure 1 It is a flow block diagram of the synthesis method of the present invention;

[0025] Figure 2 It is a three-dimensional structure schematic diagram of the purification equipment of the present invention;

[0026] Figure 3 It is a cross-sectional view of the purification equipment of the present invention;

[0027] Figure 4 is Figure 3 an enlarged schematic view of part A in

[0028] Figure 5 is Figure 3 an enlarged schematic view of part B in

[0029] Figure 6 It is a top view of the filter column of the purification equipment of the present invention;

[0030] Figure 7 It is a bottom view of the filter column of the purification equipment of the present invention.

[0031] Reference numerals in the drawings: 1. barrel body, 2. upper cover, 3. filter column, 4. bolt, 5. purification chamber, 6. purification hole, 7. fixed outer shell, 8. through hole, 9. hollow fiber membrane tube, 10. collection chamber, 11. docking chamber, 12. guide groove, 13. card slot, 14. positioning block one, 15. spring one, 16. positioning hole one, 17. positioning block two, 18. docking ring, 19. spring two, 20. mounting seat, 21. annular sealing ring, 22. magnet block. Detailed Embodiments

[0032] The following will describe in detail the embodiments of the present invention in conjunction with the drawings and embodiments, so as to fully understand how the present invention uses technical means to solve technical problems and achieve the realization process of technical effects and implement accordingly.

[0033] In the description of the present invention, it should be noted that for orientation terms, such as the terms "center", "horizontal", "longitudinal", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc., the indicated orientation and positional relationship are based on the orientation or positional relationship shown in the drawings. This is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and should not be construed as limiting the specific protection scope of the present invention.

[0034] In addition, such terms as "first" and "second" are only used for descriptive purposes and should not be construed as indicating or implying relative importance or implicitly specifying the quantity of technical features. Thus, features defined with "first" and "second" may explicitly or implicitly include one or more of such features. In the description of the present invention, the meaning of "several" is two or more, unless otherwise specifically defined.

[0035] In the present invention, unless otherwise clearly specified and defined, for the terms "assembled", "connected", and "joined", they should be understood in a broad sense. For example, it may be a fixed connection, a detachable connection, or an integral connection; it may also be a mechanical connection; it may be directly connected, or connected through an intermediate medium, and may be internally connected and communicated between two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0036] It should be understood that when used in this specification and the appended claims, the terms "comprises" and "comprising" indicate the presence of the described features, wholes, steps, operations, elements, and / or components, but do not preclude the presence or addition of one or more other features, wholes, steps, operations, elements, components, and / or their combinations.

[0037] It should also be understood that the terms used in the description of the embodiments of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the embodiments of the present invention. As used in the description of the embodiments of the present invention and the appended claims, unless the context clearly indicates otherwise, the singular forms "a", "an", and "the" are intended to include the plural forms.

[0038] Example 1

[0039] A method for synthesizing an ultraviolet absorber, the ultraviolet absorber comprising the following components by weight parts: 10 - 30 parts of monascus pigment derivative, 5 - 15 parts of organic ultraviolet absorber, 5 - 20 parts of polyurethane, 1 - 5 parts of nanomaterial, 1 - 3 parts of light stabilizer, and 30 - 60 parts of solvent.

[0040] Example 2

[0041] This example discloses a method for synthesizing an ultraviolet absorber. The ultraviolet absorber comprises the following components by weight: 10 parts of monascus pigment derivative, 7 parts of organic ultraviolet absorber, 8 parts of polyurethane, 1 part of nanomaterial, 1 part of light stabilizer, and 30 parts of solvent.

[0042] Example 3

[0043] This example discloses a method for synthesizing an ultraviolet absorber. The ultraviolet absorber comprises the following components by weight: 20 parts of monascus pigment derivative, 5 parts of organic ultraviolet absorber, 15 parts of polyurethane, 3 parts of nanomaterial, 2 parts of light stabilizer, and 40 parts of solvent.

[0044] Example 4

[0045] This example discloses a method for synthesizing an ultraviolet absorber. The ultraviolet absorber comprises the following components by weight: 30 parts of monascus pigment derivative, 15 parts of organic ultraviolet absorber, 18 parts of polyurethane, 5 parts of nanomaterial, 3 parts of light stabilizer, and 50 parts of solvent.

[0046] Example 5

[0047] This example discloses a method for synthesizing an ultraviolet absorber. The synthesis method comprises the following steps:

[0048] S1. Dissolve the alcohol-soluble monascus pigment in a mixed solvent of anhydrous methanol and ethanol with a volume ratio of 1:1, and add 5% Pd / C catalyst.

[0049] S2. Under nitrogen protection, carry out magnetic stirring reaction at 40 °C and 0.3 MPa for 8 h.

[0050] S3. Filter to remove the catalyst, concentrate the reaction solution, purify it by silica gel column chromatography, elute with ethyl acetate / petroleum ether, collect the components with ultraviolet absorption peaks at 280 - 350 nm, and concentrate and dry.

[0051] S4. Dissolve the monascus pigment derivative, organic ultraviolet absorber, and light stabilizer in an organic solvent.

[0052] S5. Add the nanomaterial and ultrasonically disperse for 20 min.

[0053] S6. Add polyurethane and amino polysiloxane microemulsion and stir for 1 h to obtain a homogeneous solution.

[0054] S7. Put the homogeneous solution into a purification device for purification and impurity removal treatment, and finally obtain the ultraviolet absorber.

[0055] Among them, the dosage of the Pd / C catalyst in S1 is 10 wt% of the raw materials.

[0056] Among them, the organic solvent in S4 is a mixture of ethanol and ethyl acetate with a volume ratio of 3:1.

[0057] Among them, the nanomaterial in S5 is nanometer TiO2 modified by a silane coupling agent, with a particle size of 20 - 50 nm.

[0058] Among them, the polyurethane in S6 is an anionic waterborne polyurethane with a molecular weight of 5000 - 10000.

[0059] In the above solution, the monascus pigment derivative is compounded with a traditional organic ultraviolet absorber (2 - phenylbenzimidazole - 5 - sulfonic acid / UV 400) to enhance the absorption efficiency through intermolecular hydrogen bonding and π - π stacking effects; the product purity is improved by optimizing the monascus pigment hydrogenation process (specific temperature / pressure / catalyst); the polyurethane - nanomaterial co - film - forming technology is adopted to solve the bottleneck problem of poor water - wash resistance of natural components.

[0060] Example 6

[0061] This example discloses a purification device, including a purification barrel; a filtering component is arranged inside the purification barrel;

[0062] The filtering component includes a number of filter columns 3; the filter column 3 includes a fixed outer shell 7 and a hollow fiber membrane tube 9, the hollow fiber membrane tube 9 is arranged inside the fixed outer shell 7, and a through - hole 8 for liquid to flow through is arranged on the fixed outer shell 7;

[0063] A purification chamber 5 and a collection chamber 10 are arranged inside the purification barrel, the purification chamber 5 is arranged above the collection chamber 10, a number of purification holes 6 are arranged inside the purification chamber 5, the filter column 3 is detachably installed inside the purification hole 6, and the inner cavity of the hollow fiber membrane tube 9 is communicated with the collection chamber 10.

[0064] Among them, the purification barrel includes a barrel body 1 and an upper cover 2, and the upper cover 2 is detachably installed at the upper end of the barrel body 1 through bolts 4.

[0065] Specifically, the specific installation method of the filter column is as follows: a plurality of installation holes for cooperating with the filter column 3 are provided on the upper cover 2, and a positioning component for axially and circumferentially positioning the filter column 3 is provided in the installation holes. Further, the positioning component includes a first spring 15 and a first positioning block 14. An installation cavity for installing the positioning component is provided on the inner circumferential wall of the installation hole. One end of the first spring 15 is fixedly connected to the bottom of the installation cavity, and the other end is fixedly connected to the first positioning block 14. The end of the first positioning block 14 away from the first spring 15 extends out of the installation cavity and into the installation hole. A first positioning hole 16 for engaging with the first positioning block 14 is provided on the outer circumferential surface of the upper end of the fixed housing 7.

[0066] Among them, in order to enable the first positioning block to be smoothly inserted into the first positioning hole, the end of the first positioning block 14 that cooperates with the first positioning hole 16 is designed to be semi-spherical.

[0067] As another embodiment of the present invention, a positioning release component is provided at the lower end of the filter column 3. When the filter column 3 needs to be replaced, the lower end of the new filter column 3 is inserted into the upper end of the old filter column 3, and the positioning release component at the lower end of the new filter column 3 can release the positioning of the positioning component on the old filter column 3. Specifically, the positioning release component includes a second positioning block 17. Both the first positioning block 14 and the second positioning block 17 are made of magnets, and the first positioning block 14 and the second positioning block 17 are arranged in a mutually repulsive manner. After the lower end of the new filter column 3 is inserted into the upper end of the old filter column 3, the repulsive force between the first positioning block 14 and the second positioning block 17 drives the first positioning block 14 to compress the first spring 15 so that the first positioning block 14 retracts into the installation cavity, and the positioning of the positioning component on the old filter column 3 is released.

[0068] In this embodiment, further, the positioning release component further includes a second spring 19. A docking ring 18 is provided at the lower end of the filter column 3. An installation seat 20 for installing the positioning release component is provided on the docking ring 18. A fixing hole is provided on the installation seat 20. One end of the second spring 19 is fixedly connected to the bottom of the fixing hole, and the other end is fixedly connected to the second positioning block 17. A docking cavity 11 having a shape adapted to that of the docking ring 18 is provided at the upper end of the filter column 3. A vertical guiding groove 12 and a horizontal clamping groove 13 are provided on the docking cavity 11. The second positioning block 17 enters the clamping groove 13 from the guiding groove 12 and is directly opposite to the first positioning block 14. The rigidity coefficient of the spring of the second spring 19 is greater than that of the first spring 15.

[0069] In the above solution, when replacing the filter column, align the positioning block 2 on the docking ring at the lower end of the new filter column with the guiding groove in the docking cavity at the upper end of the old filter column and insert it until the positioning block 2 contacts the bottom of the guiding groove. Then rotate the new positioning column so that the positioning block 2 enters the card slot and faces the positioning block 2. Since the rigidity coefficient of the spring of spring 2 19 is greater than that of spring 1 15, spring 1 is compressed, and the positioning block 1 disengages from the positioning hole 1 and retracts into the installation cavity. At the same time as the positioning of the old filter column 3 by the positioning assembly is released, the docking between the new filter column and the old filter column is completed. Then, forcefully insert the new filter column downward until the lower end of the new filter column is fitted and installed with the bottom of the purification hole, and the replacement of the filter column can be completed. Through the above solution, when the filter column of the old filter column needs to be replaced, the replacement of the filter column can be quickly completed through the above structure without disassembling the purification barrel, improving the replacement efficiency. At the same time, during the replacement process, the purification and filtration work can continue, effectively ensuring the filtration efficiency.

[0070] In this embodiment, it should be noted that the barrel of this device is made of a transparent material. When the filtration effect of the filter column in a certain purification hole decreases, its filtration ability decreases, and the liquid passing through the hollow fiber membrane tube becomes less. Therefore, the staff can see through the transparent barrel that the liquid level in this purification hole is significantly higher than the liquid levels in the other purification holes, and thus the filter column in the corresponding purification hole can be replaced.

[0071] Among them, in order for the new filter column to be able to disengage from the old filter column after being installed and enable the old filter column to fall into the collection cavity, a fitting hole cooperating with the filter group is provided at the bottom of the purification cavity 5, and a magnet block 22 is provided on the hole wall of the fitting hole. The magnet block 22 and the positioning block 2 17 are arranged in a mutually repulsive manner. When the lower end of the new filter column is inserted into the fitting hole, the magnet faces the positioning block 2 on the filter column, and the magnet generates a repulsive force on the positioning block 2, driving the positioning block 2 to compress spring 2. The positioning block 2 disengages from the card slot and retracts into the fixing part, and the old filter column disengages from the new filter column under the action of its own gravity and falls into the collection cavity.

[0072] Among them, in order to improve the sealing performance between the fitting hole and the filter column and prevent liquid from leaking from the fitting part between the fitting hole and the filter column, a ring-shaped sealing ring 21 is provided on the hole wall of the fitting hole.

[0073] The above only illustrates the best embodiments of the present invention, but it should not be construed as a limitation to the claims. The present invention is not limited to the above embodiments, and its specific structure allows changes. All changes made within the protection scope of the independent claims of the present invention are within the protection scope of the present invention.

Claims

1. A method for synthesizing an ultraviolet absorber, characterized in that: The ultraviolet absorber comprises the following components by weight: 10-30 parts of monascus pigment derivative, 5-15 parts of organic ultraviolet absorber, 5-20 parts of polyurethane, 1-5 parts of nanomaterial, 1-3 parts of light stabilizer, and 30-60 parts of solvent.

2. The synthesis method of an ultraviolet absorber according to claim 1, wherein: The ultraviolet absorber comprises the following components by weight: 10 parts of monascus pigment derivative, 7 parts of organic ultraviolet absorber, 8 parts of polyurethane, 1 part of nanomaterial, 1 part of light stabilizer, and 30 parts of solvent.

3. A method for synthesizing an ultraviolet absorber according to claim 1, characterized in that: The ultraviolet absorber comprises the following components by weight: 20 parts of monascus pigment derivative, 5 parts of organic ultraviolet absorber, 15 parts of polyurethane, 3 parts of nanomaterial, 2 parts of light stabilizer, and 40 parts of solvent.

4. A method for synthesizing an ultraviolet absorber according to claim 1, characterized in that: The ultraviolet absorber comprises the following components by weight: 30 parts of monascus pigment derivative, 15 parts of organic ultraviolet absorber, 18 parts of polyurethane, 5 parts of nanomaterial, 3 parts of light stabilizer, and 50 parts of solvent.

5. A method for synthesizing an ultraviolet absorber according to claim 1, characterized in that: The synthesis method comprises the following steps: S1. Dissolve the alcohol-soluble monascus pigment in a mixed solvent of anhydrous methanol and ethanol with a volume ratio of 1:1, and add 5% Pd / C catalyst. S2. Under nitrogen protection, carry out magnetic stirring reaction at 40 °C and 0.3 MPa for 8 h. S3. Filter to remove the catalyst, concentrate the reaction solution, purify it by silica gel column chromatography, elute with ethyl acetate / petroleum ether, collect the components with ultraviolet absorption peaks at 280-350 nm, and concentrate and dry. S4. Dissolve the monascus pigment derivative, organic ultraviolet absorber, and light stabilizer in an organic solvent. S5. Add the nanomaterial and ultrasonically disperse for 20 min. S6. Add polyurethane and amino polysiloxane microemulsion, and stir for 1 h to obtain a homogeneous solution. S7. Put the homogeneous solution into a purification device for purification and impurity removal treatment, and finally obtain the ultraviolet absorber.

6. The synthesis method of an ultraviolet absorber according to claim 5, characterized in that: The dosage of the Pd / C catalyst in S1 is 10 wt% of the raw materials.

7. A method for synthesizing an ultraviolet absorber according to claim 5, characterized in that: The organic solvent in S4 is a mixture of ethanol and ethyl acetate with a volume ratio of 3:

1.

8. A method for synthesizing an ultraviolet absorber according to claim 5, characterized in that: The nanomaterial in S5 is nanometer TiO2 modified by a silane coupling agent, with a particle size of 20-50 nm.

9. A method for synthesizing an ultraviolet absorber according to claim 5, characterized in that: The polyurethane in S6 is an anionic aqueous polyurethane with a molecular weight of 5000-10000.

10. A method for synthesizing an ultraviolet absorber according to claim 5, characterized in that: The purification device in S7 includes a purification barrel; a filtration component is arranged in the purification barrel; the filtration component includes a plurality of filter columns; each filter column includes a fixed outer shell and a hollow fiber membrane tube, the hollow fiber membrane tube is arranged in the fixed outer shell, and a through hole for liquid to flow through is arranged on the fixed outer shell; a purification chamber and a collection chamber are arranged in the purification barrel, the purification chamber is arranged above the collection chamber, a plurality of purification holes are arranged in the purification chamber, the filter columns are detachably installed in the purification holes, and the inner cavity of the hollow fiber membrane tube is communicated with the collection chamber.

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