CN112708121A - Preparation method of nano-antimony composite catalyst for PET polymerization - Google Patents
Preparation method of nano-antimony composite catalyst for PET polymerization Download PDFInfo
- Publication number
- CN112708121A CN112708121A CN202011575758.XA CN202011575758A CN112708121A CN 112708121 A CN112708121 A CN 112708121A CN 202011575758 A CN202011575758 A CN 202011575758A CN 112708121 A CN112708121 A CN 112708121A
- Authority
- CN
- China
- Prior art keywords
- antimony
- nano
- catalyst
- palygorskite clay
- composite catalyst
- 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.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
- C08G63/86—Germanium, antimony, or compounds thereof
- C08G63/866—Antimony or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/83—Alkali metals, alkaline earth metals, beryllium, magnesium, copper, silver, gold, zinc, cadmium, mercury, manganese, or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/84—Boron, aluminium, gallium, indium, thallium, rare-earth metals, or compounds thereof
Abstract
The invention discloses a preparation method of a nano antimony-based composite catalyst for PET polymerization. The preparation method mainly uses antimony trichloride as a raw material, and high-purity nano antimony trioxide is obtained through solvothermal method and alcoholysis; the novel nano-antimony composite catalyst for PET polymerization is prepared by taking palygorskite as a carrier and controlling process parameters to enable nano-antimony trioxide to be adsorbed on the surface of the palygorskite. The technical scheme of the invention improves the activity of the antimony-based catalyst, develops a novel nanometer antimony-based polyester catalyst product with stable antimony content and less impurity components, and has great popularization and application values in the polyester industry. On the premise of ensuring good catalytic activity, the production cost of the polyester catalyst is reduced, and the economic benefit is improved; meanwhile, the utilization rate of antimony in the catalyst is improved, the content of antimony is reduced, the harm to the environment caused by using the catalyst in the PET synthesis process is effectively reduced, and the catalyst has good economic and social benefits.
Description
Technical Field
The invention relates to a preparation method of a composite catalyst for PET polymerization, in particular to a preparation method of a nano antimony-based composite catalyst for PET polymerization, and belongs to the technical field of nano composite material preparation.
Background
Polyester is a general name of polymers obtained by polycondensing polyol and polybasic acid, is a high molecular material with excellent chemical and physical properties and wide application, and becomes the variety with the largest yield in synthetic fibers. The polyester catalyst not only influences the speed of esterification and polycondensation reaction in the production process of PET, but also has obvious influence on side reaction, thermal stability and product color.
However, at present, due to the safety and sanitation and environmental problems of using antimony compounds, it is desired to reduce the use of antimony compounds or to make polyester catalysts available as a substitute for antimony compounds. Meanwhile, compounds such as germanium and titanium are themselves extremely expensive, and although the polyester produced as a catalyst is satisfactory in terms of transparency, safety, hygiene and the like, it inevitably causes an increase in cost. The composite catalyst for PET polymerization is a composite catalyst formed by compounding various metal compounds with catalytic activity with organic matters and inorganic matters, can overcome the defects of the existing raw materials to a certain extent, can achieve the purposes of improving the polyester polycondensation reaction rate and improving the quality of polyester products, and is one of the main research directions of the existing novel polyester catalysts. In the field of preparation of composite catalyst for PET polymerization, Chinese patent (CN 102977353A) "AlOOH catalyst for polyester polycondensation and its preparation method" sodium aluminate is used as raw material, and AlOOH or AlOOH and Al are prepared by hydrolysis2O3The mixture nano-catalyst has higher catalytic activity; chinese patent (CN 108484895B) "a phosphorus-titanium composite polyester catalyst and its preparation method" the catalyst prepared by using central titanium atom, phosphonate substituent group and chelate ring as molecular structure components and bonding the chelate ring and the central titanium atom through titanium-oxygen bond has good hydrolysis resistance and dispersibility in ethylene glycol, and also has excellent catalytic activity and selectivity; inThe national patent (CN 110054763B) discloses a titanium germanium composite catalyst for polyester synthesis and application thereof, wherein a sol-gel method is adopted, mixed sol of titanium dioxide and germanium dioxide is dropwise added into a complexing agent aqueous solution, the obtained composite catalyst has excellent stability and activity, and side reactions in the polyester synthesis are effectively inhibited; chinese patent (CN 103435793A) "a polyester catalyst and its preparation method and application" disclose a preparation method of homogeneous solution catalyst by mixing and reacting antimony compound, one of dibasic organic acid or its glycol vinegar, lactic acid and glycol, its synthetic process is simple, easy to operate, with low costs, can omit the heating modulation heat preservation process using solid antimony catalyst, have better market prospects; the overseas patent (WO 2013182013A1) "PREPARATION METHOD OF POLYESTER SYNTHESIS CATALYST" adopts titanium-containing compound, silicon-containing compound and tin-containing compound as raw materials to prepare the high-activity COMPOSITE CATALYST for POLYESTER SYNTHESIS, and has obvious catalytic action on POLYESTER polymerization reaction. At present, no relevant process technology for preparing the nano-antimony composite catalyst for PET polymerization by using palygorskite as a polyester catalyst carrier appears.
The application provides a method for preparing a nano-antimony composite catalyst for PET polymerization by using palygorskite as a carrier and controlling process parameters. The antimony polyester catalyst with stable antimony content and less impurity components is developed in the process of efficiently fixing the heavy metal antimony in the polyester catalyst, and has important economic and social benefits.
Disclosure of Invention
The invention aims to solve the problems that the prior process for preparing the nano-antimony-based composite catalyst is complex, the cost is high, antimony in a polyester product is easy to precipitate, the utilization rate of antimony in the antimony-based polyester catalyst is low and the like, and provides a preparation method of the nano-antimony-based composite catalyst for PET polymerization.
In order to achieve the purpose, the technical scheme of the invention comprises the following steps:
1. a preparation method of a nano antimony composite catalyst for PET polymerization is characterized by comprising the following steps:
1) weighing a certain amount of antimony trichloride, dissolving the antimony trichloride in 30.0mL of absolute ethanol, stirring for 20min at the room temperature at 300r/min, and adjusting the pH value to 8-9 by using an alkali solution to form an antimony trichloride alkali solution;
2) carrying out alcoholysis reaction on the antimony trichloride aqueous alkali obtained in the step 1) at 120 ℃ for 15h, cooling to room temperature, carrying out suction filtration, washing, and drying at 60 ℃ for 2h to obtain micron antimony trioxide;
3) dissolving the micron antimony trioxide obtained in the step 2) in 40.0mL of 50% ethanol solution, reacting for 1h at 110 ℃, performing ultrasonic treatment for 0.5h, adding 5.0mL of polyethylene glycol-400, performing ultrasonic treatment for 1h, performing suction filtration and washing for 4 times, drying for 3.5h at 65 ℃, and grinding to obtain nanometer antimony trioxide;
4) weighing 0.10-1.00g of activated palygorskite clay, and placing the palygorskite clay in 40.0mL of absolute ethyl alcohol for ultrasonic dispersion for 0.5h to obtain a uniformly dispersed palygorskite clay suspension;
5) dissolving the nano antimony trioxide obtained in the step 3) in 20.0mL of absolute ethyl alcohol, slowly dropwise adding the nano antimony trioxide into the uniformly dispersed palygorskite clay suspension obtained in the step 4) under magnetic stirring, and slowly dropwise adding 10.0mL of deionized water to form a uniform nano antimony trioxide and palygorskite clay crystal mixed solution;
6) placing the uniform mixed solution of the nano antimony trioxide and the palygorskite clay crystal obtained in the step 5) in a water bath kettle at the temperature of 25-65 ℃ for reaction for 2-8h, performing suction filtration, alternately cleaning for 4 times by using absolute ethyl alcohol and deionized water, performing vacuum drying for 5-20h at the temperature of 65 ℃, and grinding to obtain the nano antimony composite catalyst for PET polymerization.
The alkali solution is one of 5-6mol/L sodium hydroxide solution or 1-2mol/L ammonia water.
The preparation method of the activated palygorskite clay comprises the following steps: weighing 50.0g of palygorskite clay, dispersing in 700.0mL of deionized water, taking supernatant, ultrasonically dispersing for 1H, adding 250.0mL of 30% H2O2Adding 250.0mL of 1.0mol/L HCl solution after no bubbles are generated in the solution, ultrasonically dispersing for 1h, washing and centrifuging, drying for 36h under vacuum at 75 ℃, and grinding to obtain the activated palygorskite clay.
The amount of antimony trichloride is 4.0g or 5.1 g.
Compared with the background art, the invention has the beneficial effects that:
the invention takes the antimony trichloride as the raw material, obtains the high-purity nanometer antimony trioxide by the solvothermal method, has simple preparation process, low cost and high efficiency, and is beneficial to large-scale production; meanwhile, the used carrier palygorskite has wide sources, belongs to a natural water-containing nano material of magnesium aluminum silicate, can adsorb nano antimony trioxide by controlling process parameters, opens up a new path for efficiently fixing heavy metal antimony in polyester, provides a new method for preparing a novel nano antimony system composite catalyst for PET polymerization, and has good economic and social benefits.
Drawings
FIG. 1 is an FESEM photograph of a nano-antimony-based composite catalyst (d) for PET polymerization prepared in example 4.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1:
1) weighing 5.1g of antimony trichloride, dissolving the antimony trichloride in 30.0mL of absolute ethanol, stirring for 20min at the room temperature at 300r/min, and adjusting the pH value to 8 by using 5mol/L sodium hydroxide solution to form an antimony trichloride alkali solution;
2) carrying out alcoholysis reaction on the antimony trichloride aqueous alkali obtained in the step 1) at 120 ℃ for 15h, cooling to room temperature, carrying out suction filtration, washing, and drying at 60 ℃ for 2h to obtain micron antimony trioxide;
3) dissolving the micron antimony trioxide obtained in the step 2) in 40.0mL of 50% ethanol solution, reacting for 1h at 110 ℃, performing ultrasonic treatment for 0.5h, adding 5.0mL of polyethylene glycol-400, performing ultrasonic treatment for 1h, performing suction filtration and washing for 4 times, drying for 3.5h at 65 ℃, and grinding to obtain nanometer antimony trioxide;
4) weighing 1.0g of activated palygorskite clay, and placing the palygorskite clay in 40.0mL of absolute ethyl alcohol for ultrasonic dispersion for 0.5h to obtain a uniformly dispersed palygorskite clay suspension;
5) dissolving the nano antimony trioxide obtained in the step 3) in 20.0mL of absolute ethyl alcohol, slowly dropwise adding the nano antimony trioxide into the uniformly dispersed palygorskite clay suspension obtained in the step 4) under magnetic stirring, and slowly dropwise adding 10.0mL of deionized water to form a uniform nano antimony trioxide and palygorskite clay crystal mixed solution;
6) placing the uniform mixed solution of the nano antimony trioxide and the palygorskite clay crystal obtained in the step 5) in a water bath kettle at 25 ℃ for reaction for 8 hours, then carrying out suction filtration, alternately cleaning with absolute ethyl alcohol and deionized water for 4 times, carrying out vacuum drying at 65 ℃ for 20 hours, and grinding to obtain the nano antimony composite catalyst (a) for PET polymerization.
Example 2:
1) weighing 5.1g of antimony trichloride, dissolving the antimony trichloride in 30.0mL of absolute ethanol, stirring at 300r/min for 20min at room temperature, and adjusting the pH value to 8 by using 6mol/L sodium hydroxide solution to form an antimony trichloride alkali solution;
2) carrying out alcoholysis reaction on the antimony trichloride aqueous alkali obtained in the step 1) at 120 ℃ for 15h, cooling to room temperature, carrying out suction filtration, washing, and drying at 60 ℃ for 2h to obtain micron antimony trioxide;
3) dissolving the micron antimony trioxide obtained in the step 2) in 40.0mL of 50% ethanol solution, reacting for 1h at 110 ℃, performing ultrasonic treatment for 0.5h, adding 5.0mL of polyethylene glycol-400, performing ultrasonic treatment for 1h, performing suction filtration and washing for 4 times, drying for 3.5h at 65 ℃, and grinding to obtain nanometer antimony trioxide;
4) weighing 0.5g of activated palygorskite clay, and placing the palygorskite clay in 40.0mL of absolute ethyl alcohol for ultrasonic dispersion for 0.5h to obtain a uniformly dispersed palygorskite clay suspension;
5) dissolving the nano antimony trioxide obtained in the step 3) in 20.0mL of absolute ethyl alcohol, slowly dropwise adding the nano antimony trioxide into the uniformly dispersed palygorskite clay suspension obtained in the step 4) under magnetic stirring, and slowly dropwise adding 10.0mL of deionized water to form a uniform nano antimony trioxide and palygorskite clay crystal mixed solution;
6) placing the uniform mixed solution of the nano antimony trioxide and the palygorskite clay crystal obtained in the step 5) in a 45 ℃ water bath kettle for reaction for 4 hours, then carrying out suction filtration, alternately cleaning for 4 times by using absolute ethyl alcohol and deionized water, carrying out vacuum drying for 10 hours at 65 ℃, and grinding to obtain the nano antimony composite catalyst (b) for PET polymerization.
Example 3:
1) weighing 5.1g of antimony trichloride, dissolving the antimony trichloride in 30.0mL of absolute ethanol, stirring for 20min at the room temperature at 300r/min, and adjusting the pH value to 9 by using 6mol/L sodium hydroxide solution to form an antimony trichloride alkali solution;
2) carrying out alcoholysis reaction on the antimony trichloride aqueous alkali obtained in the step 1) at 120 ℃ for 15h, cooling to room temperature, carrying out suction filtration, washing, and drying at 60 ℃ for 2h to obtain micron antimony trioxide;
3) dissolving the micron antimony trioxide obtained in the step 2) in 40.0mL of 50% ethanol solution, reacting for 1h at 110 ℃, performing ultrasonic treatment for 0.5h, adding 5.0mL of polyethylene glycol-400, performing ultrasonic treatment for 1h, performing suction filtration and washing for 4 times, drying for 3.5h at 65 ℃, and grinding to obtain nanometer antimony trioxide;
4) weighing 0.25g of activated palygorskite clay, and placing the palygorskite clay in 40.0mL of absolute ethyl alcohol for ultrasonic dispersion for 0.5h to obtain a uniformly dispersed palygorskite clay suspension;
5) dissolving the nano antimony trioxide obtained in the step 3) in 20.0mL of absolute ethyl alcohol, slowly dropwise adding the nano antimony trioxide into the uniformly dispersed palygorskite clay suspension obtained in the step 4) under magnetic stirring, and slowly dropwise adding 10.0mL of deionized water to form a uniform nano antimony trioxide and palygorskite clay crystal mixed solution;
6) placing the uniform mixed solution of the nano antimony trioxide and the palygorskite clay crystal obtained in the step 5) in a 65 ℃ water bath kettle for reaction for 2 hours, then carrying out suction filtration, alternately cleaning for 4 times by using absolute ethyl alcohol and deionized water, carrying out vacuum drying for 5 hours at 65 ℃, and grinding to obtain the nano antimony composite catalyst (c) for PET polymerization.
Example 4:
1) weighing 4.0g of antimony trichloride, dissolving the antimony trichloride in 30.0mL of absolute ethanol, stirring for 20min at the room temperature at 300r/min, and adjusting the pH value to 9 by using 1mol/L ammonia water to form an antimony trichloride alkali solution;
2) carrying out alcoholysis reaction on the antimony trichloride aqueous alkali obtained in the step 1) at 120 ℃ for 15h, cooling to room temperature, carrying out suction filtration, washing, and drying at 60 ℃ for 2h to obtain micron antimony trioxide;
3) dissolving the micron antimony trioxide obtained in the step 2) in 40.0mL of 50% ethanol solution, reacting for 1h at 110 ℃, performing ultrasonic treatment for 0.5h, adding 5.0mL of polyethylene glycol-400, performing ultrasonic treatment for 1h, performing suction filtration and washing for 4 times, drying for 3.5h at 65 ℃, and grinding to obtain nanometer antimony trioxide;
4) weighing 0.1g of activated palygorskite clay, and placing the palygorskite clay in 40.0mL of absolute ethyl alcohol for ultrasonic dispersion for 0.5h to obtain a uniformly dispersed palygorskite clay suspension;
5) dissolving the nano antimony trioxide obtained in the step 3) in 20.0mL of absolute ethyl alcohol, slowly dropwise adding the nano antimony trioxide into the uniformly dispersed palygorskite clay suspension obtained in the step 4) under magnetic stirring, and slowly dropwise adding 10.0mL of deionized water to form a uniform nano antimony trioxide and palygorskite clay crystal mixed solution;
6) placing the uniform mixed solution of the nano antimony trioxide and the palygorskite clay crystal obtained in the step 5) in a water bath kettle at 25 ℃ for reaction for 4 hours, then carrying out suction filtration, alternately cleaning with absolute ethyl alcohol and deionized water for 4 times, carrying out vacuum drying at 65 ℃ for 10 hours, and grinding to obtain the nano antimony composite catalyst (d) for PET polymerization.
Example 5:
1) weighing 4.0g of antimony trichloride, dissolving the antimony trichloride in 30.0mL of absolute ethanol, stirring for 20min at the room temperature at 300r/min, and adjusting the pH value to 9 by using 2mol/L ammonia water to form an antimony trichloride alkali solution;
2) carrying out alcoholysis reaction on the antimony trichloride aqueous alkali obtained in the step 1) at 120 ℃ for 15h, cooling to room temperature, carrying out suction filtration, washing, and drying at 60 ℃ for 2h to obtain micron antimony trioxide;
3) dissolving the micron antimony trioxide obtained in the step 2) in 40.0mL of 50% ethanol solution, reacting for 1h at 110 ℃, performing ultrasonic treatment for 0.5h, adding 5.0mL of polyethylene glycol-400, performing ultrasonic treatment for 1h, performing suction filtration and washing for 4 times, drying for 3.5h at 65 ℃, and grinding to obtain nanometer antimony trioxide;
4) weighing 1.0g of activated palygorskite clay, and placing the palygorskite clay in 40.0mL of absolute ethyl alcohol for ultrasonic dispersion for 0.5h to obtain a uniformly dispersed palygorskite clay suspension;
5) dissolving the nano antimony trioxide obtained in the step 3) in 20.0mL of absolute ethyl alcohol, slowly dropwise adding the nano antimony trioxide into the uniformly dispersed palygorskite clay suspension obtained in the step 4) under magnetic stirring, and slowly dropwise adding 10.0mL of deionized water to form a uniform nano antimony trioxide and palygorskite clay crystal mixed solution;
6) placing the uniform mixed solution of the nano antimony trioxide and the palygorskite clay crystal obtained in the step 5) in a 65 ℃ water bath kettle for reaction for 2 hours, then carrying out suction filtration, alternately cleaning for 4 times by using absolute ethyl alcohol and deionized water, carrying out vacuum drying for 5 hours at 65 ℃, and grinding to obtain the nano antimony composite catalyst (e) for PET polymerization.
The morphology and size of the nano antimony-based composite catalyst for PET polymerization prepared in examples 1, 2, 3, 4 and 5 were observed and measured. Table 1 shows the results of the morphology and size measurements of the nano-antimony-based composite catalysts for PET polymerization prepared in examples 1, 2, 3, 4 and 5. From the data in table 1, it can be seen that: the shape and the size of the nano antimony-based composite catalyst for PET polymerization prepared by the technical scheme of the invention meet the requirements of polyester catalysts. Wherein, the shape of the nano antimony composite catalyst for PET polymerization is cubic crystal fiber or spherical particle fiber, and the average particle diameter is 10-400.0 nm.
As shown in fig. 1, from the FESEM photograph of the nano antimony-based composite catalyst for PET polymerization (d) prepared in example 4, it can be seen that: in the PET polymerization nanometer antimony system composite catalyst (d), a large amount of approximately spherical antimony trioxide is mutually bonded and uniformly and tightly loaded on the fibrous palygorskite.
TABLE 1
The foregoing lists merely illustrate specific embodiments of the invention. The present invention is not limited to the above embodiments, and many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (4)
1. A preparation method of a nano antimony composite catalyst for PET polymerization is characterized by comprising the following steps:
1) weighing a certain amount of antimony trichloride, dissolving the antimony trichloride in 30.0mL of absolute ethanol, stirring for 20min at the room temperature at 300r/min, and adjusting the pH value to 8-9 by using an alkali solution to form an antimony trichloride alkali solution;
2) carrying out alcoholysis reaction on the antimony trichloride aqueous alkali obtained in the step 1) at 120 ℃ for 15h, cooling to room temperature, carrying out suction filtration, washing, and drying at 60 ℃ for 2h to obtain micron antimony trioxide;
3) dissolving the micron antimony trioxide obtained in the step 2) in 40.0mL of 50% ethanol solution, reacting for 1h at 110 ℃, performing ultrasonic treatment for 0.5h, adding 5.0mL of polyethylene glycol-400, performing ultrasonic treatment for 1h, performing suction filtration and washing for 4 times, drying for 3.5h at 65 ℃, and grinding to obtain nanometer antimony trioxide;
4) weighing 0.10-1.00g of activated palygorskite clay, and placing the palygorskite clay in 40.0mL of absolute ethyl alcohol for ultrasonic dispersion for 0.5h to obtain a uniformly dispersed palygorskite clay suspension;
5) dissolving the nano antimony trioxide obtained in the step 3) in 20.0mL of absolute ethyl alcohol, slowly dropwise adding the nano antimony trioxide into the uniformly dispersed palygorskite clay suspension obtained in the step 4) under magnetic stirring, and slowly dropwise adding 10.0mL of deionized water to form a uniform nano antimony trioxide and palygorskite clay crystal mixed solution;
6) placing the uniform mixed solution of the nano antimony trioxide and the palygorskite clay crystal obtained in the step 5) in a water bath kettle at the temperature of 25-65 ℃ for reaction for 2-8h, performing suction filtration, alternately cleaning for 4 times by using absolute ethyl alcohol and deionized water, performing vacuum drying for 5-20h at the temperature of 65 ℃, and grinding to obtain the nano antimony composite catalyst for PET polymerization.
2. The method for preparing the nano antimony-based composite catalyst for PET polymerization according to claim 1, wherein the method comprises the following steps: the alkali solution is one of 5-6mol/L sodium hydroxide solution or 1-2mol/L ammonia water.
3. The method for preparing the nano antimony-based composite catalyst for PET polymerization according to claim 1, wherein the method comprises the following steps: the preparation method of the activated palygorskite clay comprises weighing 50.0g of palygorskite clay, dispersing in 700.0mL of deionized water, taking supernatant, ultrasonically dispersing for 1H, adding 250.0mL of 30% H2O2Adding 250.0mL of 1.0mol/L HCl solution after no bubbles are generated in the solution, ultrasonically dispersing for 1h, washing and centrifuging, drying for 36h under vacuum at 75 ℃, and grinding to obtain the activated palygorskite clay.
4. The method for preparing the nano antimony-based composite catalyst for PET polymerization according to claim 1, wherein the method comprises the following steps: the amount of antimony trichloride is 4.0g or 5.1 g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011575758.XA CN112708121A (en) | 2020-12-28 | 2020-12-28 | Preparation method of nano-antimony composite catalyst for PET polymerization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011575758.XA CN112708121A (en) | 2020-12-28 | 2020-12-28 | Preparation method of nano-antimony composite catalyst for PET polymerization |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112708121A true CN112708121A (en) | 2021-04-27 |
Family
ID=75545689
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011575758.XA Pending CN112708121A (en) | 2020-12-28 | 2020-12-28 | Preparation method of nano-antimony composite catalyst for PET polymerization |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112708121A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113321240A (en) * | 2021-05-20 | 2021-08-31 | 浙江理工大学 | Preparation method of high-dispersity nano antimony trioxide |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565500A (en) * | 2008-04-23 | 2009-10-28 | 中国科学院化学研究所 | Polyester/clay nanometer composite material, special catalyst thereof and methods for preparing polyester/clay nanometer composite material and special catalyst thereof |
| US20090286917A1 (en) * | 2007-12-20 | 2009-11-19 | Surbhi Mahajan | Improved catalyst system for polyester nanocomposites |
| CN101899201A (en) * | 2010-07-28 | 2010-12-01 | 江阴济化新材料有限公司 | Method for preparing PET (Polyethylene Terephthalate) engineering plastic particle of attapulgite fast crystallization |
| CN102627759A (en) * | 2012-03-21 | 2012-08-08 | 东华大学 | Polyester catalyst with attapulgite as carrier, preparation thereof and application thereof |
| CN109400856A (en) * | 2018-09-26 | 2019-03-01 | 浙江恒澜科技有限公司 | A method of catalyzing and synthesizing the polypropylene terephthalate of high inherent viscosity and good form and aspect using metal composite catalyst |
-
2020
- 2020-12-28 CN CN202011575758.XA patent/CN112708121A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090286917A1 (en) * | 2007-12-20 | 2009-11-19 | Surbhi Mahajan | Improved catalyst system for polyester nanocomposites |
| CN101565500A (en) * | 2008-04-23 | 2009-10-28 | 中国科学院化学研究所 | Polyester/clay nanometer composite material, special catalyst thereof and methods for preparing polyester/clay nanometer composite material and special catalyst thereof |
| CN101899201A (en) * | 2010-07-28 | 2010-12-01 | 江阴济化新材料有限公司 | Method for preparing PET (Polyethylene Terephthalate) engineering plastic particle of attapulgite fast crystallization |
| CN102627759A (en) * | 2012-03-21 | 2012-08-08 | 东华大学 | Polyester catalyst with attapulgite as carrier, preparation thereof and application thereof |
| CN109400856A (en) * | 2018-09-26 | 2019-03-01 | 浙江恒澜科技有限公司 | A method of catalyzing and synthesizing the polypropylene terephthalate of high inherent viscosity and good form and aspect using metal composite catalyst |
Non-Patent Citations (1)
| Title |
|---|
| 杜兆芳等: "超声场醇盐水解三氧化二锑颗粒的制备与表征", 《材料科学与工艺》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113321240A (en) * | 2021-05-20 | 2021-08-31 | 浙江理工大学 | Preparation method of high-dispersity nano antimony trioxide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110004521B (en) | Preparation method of spinnable silicon-aluminum sol | |
| CN108273564B (en) | Composite visible light photocatalyst Ag2CO3/TiO2/UiO-66-(COOH)2Preparation method and application thereof | |
| CN102145280B (en) | Method for preparing rice hull active carbon/silicon dioxide/titanium dioxide composite material | |
| TW201119947A (en) | Stable nano titania sols and a process for their production | |
| CN101773852A (en) | Supported ionic liquid catalyst and preparation method and application thereof | |
| CN108295830B (en) | TiO with 001, 101 crystal face exposed2Sepiolite composite gel and preparation method thereof | |
| CN1908291A (en) | TiO2 nano-sized hydrosol, preparation process thereof and textile finish method | |
| CN108077308A (en) | A kind of antimicrobial nano titania-silica aqueous dispersion of nucleocapsid | |
| CN110240723B (en) | Ultraviolet high-shielding cellulose membrane and preparation method and application thereof | |
| CN112708121A (en) | Preparation method of nano-antimony composite catalyst for PET polymerization | |
| CN103007912A (en) | One-dimensional nanometer titania photocatalyst with mica serving as support and preparation method thereof | |
| CN104998629B (en) | A kind of core shell structure SiO2‑TiO2Composite nano materials and its preparation method and application | |
| CN115716918A (en) | Method for preparing metal-organic framework material by ball milling-solution blending | |
| CN103789819A (en) | Preparation method of fibrous alkali magnesium sulfate whisker | |
| CN1616518A (en) | Process for in-situ quiclely preparing crystalline polyester using nano silicon dioxide | |
| CN101774807A (en) | Preparation method of zirconium carbide micropowder | |
| CN108295897B (en) | A kind of compounded visible light photocatalyst Ag2CO3/TiO2/UIO-66-(COOH)2And organic matter degradation application | |
| CN102443154A (en) | Aerogel catalyst and preparation method thereof | |
| CN116282049A (en) | Preparation method of controllable ordered mesoporous silica microsphere | |
| CN103693689B (en) | Utilize kind of crystallization synthesis of nano t-ZrO between water-oil interface 2the method of particle | |
| CN109369882A (en) | A kind of titanium deoxid film preparation method based on nano-fluid | |
| CN112011039A (en) | Water-soluble polymer modifier with polyester structure for calcium carbonate surface modification and preparation method thereof | |
| CN111704852A (en) | Ag-TiO2Modified polyurethane antibacterial paint and preparation method thereof | |
| CN107344118B (en) | TiO with controllable surface growth morphology for preparing porous resin microspheres2Method (2) | |
| CN106345443A (en) | Photocatalysis material with nano TiO2 loaded on kieselguhr white carbon black used as carrier and preparation method of photocatalysis material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210427 |
|
| WD01 | Invention patent application deemed withdrawn after publication |