CN115746284A - Method for removing residual titanate catalyst in light stabilizer 622 - Google Patents
Method for removing residual titanate catalyst in light stabilizer 622 Download PDFInfo
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- CN115746284A CN115746284A CN202211473767.7A CN202211473767A CN115746284A CN 115746284 A CN115746284 A CN 115746284A CN 202211473767 A CN202211473767 A CN 202211473767A CN 115746284 A CN115746284 A CN 115746284A
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- China
- Prior art keywords
- light stabilizer
- activated carbon
- titanate catalyst
- residual
- titanate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 239000004611 light stabiliser Substances 0.000 title claims abstract description 52
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000003054 catalyst Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 89
- 238000001914 filtration Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 16
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical group [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 abstract description 6
- 239000010936 titanium Substances 0.000 abstract description 6
- 230000007062 hydrolysis Effects 0.000 abstract 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract 2
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 8
- 150000001412 amines Chemical class 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 3
- 150000002148 esters Chemical group 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- YLCCMQJTYLKSTK-UHFFFAOYSA-N 2-(1-hydroxypiperidin-2-yl)ethanol Chemical compound OCCC1CCCCN1O YLCCMQJTYLKSTK-UHFFFAOYSA-N 0.000 description 1
- MUXOBHXGJLMRAB-UHFFFAOYSA-N Dimethyl succinate Chemical compound COC(=O)CCC(=O)OC MUXOBHXGJLMRAB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Catalysts (AREA)
Abstract
The invention discloses a method for removing a residual titanate catalyst in a light stabilizer 622, which comprises the steps of simultaneously hydrolyzing and adsorbing the residual titanate catalyst in the light stabilizer 622 by using treated activated carbon, adsorbing a hydrolysis product of the titanate catalyst on the catalyst, and separating and removing the hydrolysis product from the light stabilizer 622 through subsequent filtration, wherein titanium in the treated light stabilizer 622 is remained within 100 ppm.
Description
Technical Field
The invention belongs to the technical field of chemical purification, and particularly relates to a method for removing a residual titanate catalyst in a light stabilizer 622.
Background
The hindered amine light stabilizer 622 is an efficient and high molecular weight type hindered amine light stabilizer initiated by Ciba-Geigy corporation in the beginning of the 80 th century in Switzerland, due to the excellent performance of the hindered amine light stabilizer 622, the hindered amine light stabilizer 622 attracts domestic wide attention in recent years, and a plurality of scientific research units and production enterprises research the synthesis of the hindered amine light stabilizer 622.
At present, the mainstream method for producing the light stabilizer 622 domestically and internationally is an ester exchange method, and a product is obtained by taking hydroxyethyl piperidinol and dimethyl succinate as raw materials through ester exchange reaction; the catalyst commonly used in the ester exchange method is titanate catalyst which is uniformly dispersed in the system and is difficult to remove. In subsequent application of products, the catalyst residue may cause red, turbid and the like, and the use and performance of the products are seriously influenced.
Disclosure of Invention
In order to solve the problems, the invention discloses a method for removing a residual titanate catalyst in a light stabilizer 622.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method of removing residual titanate catalyst from light stabilizer 622, the method comprising the steps of:
step (1): placing the activated carbon in a steam atmosphere, and keeping the activated carbon at normal temperature for 3 hours to ensure that the activated carbon fully absorbs moisture to obtain treated activated carbon;
step (2): putting the light stabilizer 622 into a treatment kettle, raising the temperature of the kettle to 140-160 ℃, and stirring to melt the light stabilizer 622 into a liquid state;
and (3): adding the activated carbon treated in the step (1) into the treatment kettle in the step (2), and stirring at a constant temperature;
filtering the materials in the treatment kettle by using filter paper with the precision of 2-10 mu m, removing the activated carbon, and detecting the water content of the treated activated carbon by using a drying method to obtain a light stabilizer 622 after the residual titanate catalyst is removed; the pH value of the activated carbon is 2 to 4, and the particle size of the activated carbon is 1 to 1.5mm.
Further, the weight of the activated carbon is 1% -3% of that of the light stabilizer 622.
Further, the water content of the activated carbon after the treatment in the step (1) is 10 to 20 percent.
Further, the stirring time in the step (3) is 2 to 4h.
Further, the temperature of the heat preservation stirring in the step (3) is 140-160 ℃.
Further, in step (4), the titanate catalyst is tetraethyl titanate.
The beneficial effects of the invention are as follows:
1. according to the invention, the titanate catalyst added in the reaction process of the light stabilizer 622 can be effectively removed;
2. according to the invention, the active carbon which adsorbs water in advance is used for treating the material, the titanate catalyst can be rapidly hydrolyzed and adsorbed on the active carbon after contacting the active carbon, and the titanate catalyst can be removed by filtration.
3. The light stabilizer 622 treated by the method cannot be red and cloudy due to the residue of the titanate catalyst in the subsequent application process.
Drawings
FIG. 1 shows the results of the detection of residual titanium in the light stabilizer 622 before treatment by the method of the present invention;
FIG. 2 shows the results of detection of residual titanium using the light stabilizer 622 after the treatment of example 1;
FIG. 3 shows the results of the detection of residual titanium using the light stabilizer 622 after the treatment of example 2;
FIG. 4 shows the results of the detection of residual titanium using the light stabilizer 622 after the treatment of example 3;
FIG. 5 shows the results of detection of residual titanium using the light stabilizer 622 after the treatment of example 4.
Detailed Description
The present invention will be further illustrated with reference to the accompanying drawings and detailed description, which will be understood as being illustrative only and not limiting in scope.
Example 1
Weighing 1g of activated carbon with the pH of 2-4 and the particle size of 1-1.5 mm, placing the activated carbon in a water vapor atmosphere, keeping the activated carbon at normal temperature for 3 hours to enable the activated carbon to fully absorb water, and detecting the water content to be 13.3% by using a drying method;
weighing 100g of light stabilizer 622, as shown in figure 1, the titanate catalyst is tetraethyl titanate; adding a light stabilizer 622 into a treatment kettle when the titanium residue is 865.9ppm, raising the temperature of the treatment kettle to 140 ℃, and melting the light stabilizer 622 into a liquid state; opening stirring, putting the treated activated carbon into a treatment kettle, preserving heat at 140 ℃ and stirring for 3 hours; filtration gave the light stabilizer 622 after removal of the residual titanate catalyst, see FIG. 2, with a titanium residue of 80.49ppm.
Example 2
Weighing 2g of activated carbon with the pH of 2-4 and the particle size of 1-1.5 mm, placing the activated carbon in a water vapor atmosphere, keeping the activated carbon at normal temperature for 3 hours to enable the activated carbon to fully absorb water, and detecting the water content to be 16.8% by using a drying method;
weighing 100g of light stabilizer 622, and taking titanate catalyst as tetraethyl titanate; the titanium residue was 865.9ppm, as shown in fig. 1, the light stabilizer 622 was put into the treatment kettle, the kettle temperature was raised to 140 ℃, and the light stabilizer 622 was melted into a liquid state; opening stirring, putting the treated activated carbon into a treatment kettle, preserving heat at 140 ℃ and stirring for 3 hours; filtration gave the treated light stabilizer 622, shown in FIG. 3, with a titanium residue of 57.61ppm.
Example 3
Weighing 3g of activated carbon with the pH of 2-4 and the particle size of 1-1.5 mm, placing the activated carbon in a water vapor atmosphere, keeping the activated carbon at normal temperature for 3 hours to enable the activated carbon to fully absorb water, and detecting the water content to be 15.6% by using a drying method;
weighing 100g of light stabilizer 622, as shown in figure 1, the titanate catalyst is tetraethyl titanate; adding the titanium residue of 865.9ppm into a treatment kettle, raising the temperature of a light stabilizer 622 to 150 ℃, and melting the light stabilizer 622 into a liquid state; opening stirring, putting the treated activated carbon into a treatment kettle, keeping the temperature at 150 ℃, and stirring for 3 hours; filtration gave the treated light stabilizer 622, shown in FIG. 4, with a titanium residue of 19.9ppm.
Example 4
Weighing 1g of activated carbon with the pH of 2-4 and the particle size of 1-1.5 mm, placing the activated carbon in a water vapor atmosphere, keeping the activated carbon at normal temperature for 3 hours to enable the activated carbon to fully absorb water, and detecting the water content to be 13.3% by using a drying method;
weighing 100g of light stabilizer 622, as shown in figure 1, the titanate catalyst is tetraethyl titanate; adding the titanium residue of 865.9ppm into a treatment kettle, raising the temperature of a light stabilizer 622 to 150 ℃, and melting the light stabilizer 622 into a liquid state; opening stirring, putting the treated activated carbon into a treatment kettle, keeping the temperature at 150 ℃, and stirring for 3 hours; filtration gave the treated light stabilizer 622, as shown in the figure, with a titanium residue of 84.1ppm.
It should be noted that the above-mentioned contents only illustrate the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and it is obvious to those skilled in the art that several modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations fall within the protection scope of the claims of the present invention.
Claims (6)
1. A method for removing residual titanate catalyst in light stabilizer 622, which is characterized by comprising the following steps:
step (1): placing the activated carbon in a steam atmosphere, and keeping the activated carbon at normal temperature for 3 hours to ensure that the activated carbon fully absorbs moisture to obtain treated activated carbon;
step (2): putting the light stabilizer 622 into a treatment kettle, raising the temperature of the kettle to 140-160 ℃, and stirring to melt the light stabilizer 622 into a liquid state;
and (3): adding the activated carbon treated in the step (1) into the treatment kettle in the step (2), and stirring while keeping the temperature;
and (4): filtering the materials in the treatment kettle by using filter paper with the precision of 2 to 10 mu m, removing the activated carbon, and detecting the water content of the treated activated carbon by using a drying method to obtain the light stabilizer 622 after the residual titanate catalyst is removed; the pH value of the activated carbon is 2 to 4, and the particle size of the activated carbon is 1 to 1.5mm.
2. The method for removing the residual titanate catalyst in the light stabilizer 622 according to claim 1, wherein the weight of the activated carbon is 1% to 3% of the weight of the light stabilizer 622.
3. The method for removing the residual titanate catalyst in the light stabilizer 622 according to claim 1, wherein the water content of the treated activated carbon in the step (1) is 10-20%.
4. The method for removing the residual titanate catalyst in the light stabilizer 622 according to claim 1, wherein the stirring time in the step (3) is 2 to 4h.
5. The method for removing the residual titanate catalyst in the light stabilizer 622 according to claim 1, wherein the stirring temperature in the step (3) is 140 ℃ to 160 ℃.
6. The method of claim 1, wherein the titanate catalyst is tetraethyl titanate, and the method of removing the residual titanate catalyst from the light stabilizer 622 is carried out in the presence of a solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211473767.7A CN115746284A (en) | 2022-11-23 | 2022-11-23 | Method for removing residual titanate catalyst in light stabilizer 622 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211473767.7A CN115746284A (en) | 2022-11-23 | 2022-11-23 | Method for removing residual titanate catalyst in light stabilizer 622 |
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|---|---|
| CN115746284A true CN115746284A (en) | 2023-03-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202211473767.7A Pending CN115746284A (en) | 2022-11-23 | 2022-11-23 | Method for removing residual titanate catalyst in light stabilizer 622 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58121245A (en) * | 1982-01-11 | 1983-07-19 | Sekisui Chem Co Ltd | Preparation of ester |
| CN101489971A (en) * | 2006-08-23 | 2009-07-22 | 赢创罗麦斯添加剂有限责任公司 | Process for preparing carboxylic acid derivatives |
| CN104592504A (en) * | 2015-01-21 | 2015-05-06 | 苏州飞翔新材料研究院有限公司 | Method for preparing light stabilizer 622 |
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2022
- 2022-11-23 CN CN202211473767.7A patent/CN115746284A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58121245A (en) * | 1982-01-11 | 1983-07-19 | Sekisui Chem Co Ltd | Preparation of ester |
| CN101489971A (en) * | 2006-08-23 | 2009-07-22 | 赢创罗麦斯添加剂有限责任公司 | Process for preparing carboxylic acid derivatives |
| CN104592504A (en) * | 2015-01-21 | 2015-05-06 | 苏州飞翔新材料研究院有限公司 | Method for preparing light stabilizer 622 |
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