CN115785409A - Titanium catalyst and preparation method thereof - Google Patents
Titanium catalyst and preparation method thereof Download PDFInfo
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- CN115785409A CN115785409A CN202211464328.XA CN202211464328A CN115785409A CN 115785409 A CN115785409 A CN 115785409A CN 202211464328 A CN202211464328 A CN 202211464328A CN 115785409 A CN115785409 A CN 115785409A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 59
- 239000010936 titanium Substances 0.000 title claims abstract description 49
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 229940126062 Compound A Drugs 0.000 claims abstract description 21
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 claims abstract description 21
- MMCOUVMKNAHQOY-UHFFFAOYSA-N carbonoperoxoic acid Chemical compound OOC(O)=O MMCOUVMKNAHQOY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 150000003609 titanium compounds Chemical class 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- -1 3, 5-di-tert-butyl-4-hydroxybenzyl diethyl phosphonate Chemical compound 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 13
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- RBNPOMFGQQGHHO-UHFFFAOYSA-N glyceric acid Chemical compound OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 claims description 10
- PDGXJDXVGMHUIR-UHFFFAOYSA-N 2,3-Dihydroxy-3-methylpentanoate Chemical compound CCC(C)(O)C(O)C(O)=O PDGXJDXVGMHUIR-UHFFFAOYSA-N 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- KJTLQQUUPVSXIM-UHFFFAOYSA-N mevalonic acid Chemical compound OCCC(O)(C)CC(O)=O KJTLQQUUPVSXIM-UHFFFAOYSA-N 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 abstract description 25
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract 1
- 239000012265 solid product Substances 0.000 description 12
- 229910052787 antimony Inorganic materials 0.000 description 9
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 9
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 238000005886 esterification reaction Methods 0.000 description 4
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 4
- 230000032050 esterification Effects 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 description 2
- UOXJNGFFPMOZDM-UHFFFAOYSA-N 2-[di(propan-2-yl)amino]ethylsulfanyl-methylphosphinic acid Chemical compound CC(C)N(C(C)C)CCSP(C)(O)=O UOXJNGFFPMOZDM-UHFFFAOYSA-N 0.000 description 2
- SFHYNDMGZXWXBU-LIMNOBDPSA-N 6-amino-2-[[(e)-(3-formylphenyl)methylideneamino]carbamoylamino]-1,3-dioxobenzo[de]isoquinoline-5,8-disulfonic acid Chemical compound O=C1C(C2=3)=CC(S(O)(=O)=O)=CC=3C(N)=C(S(O)(=O)=O)C=C2C(=O)N1NC(=O)N\N=C\C1=CC=CC(C=O)=C1 SFHYNDMGZXWXBU-LIMNOBDPSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000002759 woven fabric Substances 0.000 description 2
- JVYDLYGCSIHCMR-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)butanoic acid Chemical compound CCC(CO)(CO)C(O)=O JVYDLYGCSIHCMR-UHFFFAOYSA-N 0.000 description 1
- WSXIMVDZMNWNRF-UHFFFAOYSA-N antimony;ethane-1,2-diol Chemical compound [Sb].OCCO WSXIMVDZMNWNRF-UHFFFAOYSA-N 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention discloses a titanium catalyst and a preparation method thereof, wherein the titanium catalyst comprises a compound A which is a four-membered ring or a six-membered ring structure; when the compound A is of a four-membered ring structure, the structural formula is shown as a formula (1), and when the compound A is of a six-membered ring structure, the structural formula is shown as a formula (2). Also comprises a compound B, the structural formula of which is shown as the formula (3). The preparation method comprises the following steps: slowly adding a dihydroxy carboxylic acid solution into a titanium compound solution, filtering a turbid solution after the reaction is finished, and washing and drying to obtain a compound A; slowly adding the 3, 5-di-tert-butyl-4-hydroxybenzyl diethyl phosphonate solution into the titanium compound solution, filtering the turbid solution after the reaction is finished, and washing and drying to obtain a compound B; mixing the compound A and the compound B in proportion to obtain the compound. The titanium catalyst has the advantages of stable structure, simple preparation process, good dissolution in glycol, high catalytic activity and improved brightness of polyester products.
Description
Technical Field
The invention relates to a catalyst for polyester production and a preparation method thereof, in particular to a titanium catalyst and a preparation method thereof.
Background
At present, more than 90 percent of polyester production enterprises at home and abroad adopt antimony catalysts. Antimony is a heavy metal, the activity is general, the requirement of environmental protection is not met, and the antimony is easy to separate out, so that the color of the product is grey. Antimony is a heavy metal element, and in recent years, the use of antimony has been newly demanded in the european union, the united states, japan, and the like.
Compared with antimony catalysts, titanium (Ti) catalysts are environment-friendly, high in catalytic activity, small in addition amount, belong to non-heavy metal elements, are harmless to human bodies, and are considered by the scientific community as environment-friendly catalysts which are most likely to replace antimony catalysts and realize application, so that the relevant research is carried out on the titanium (Ti) catalysts from the 20 th century and the 70 th century.
Disclosure of Invention
The invention aims to: the invention aims to provide a titanium catalyst with high catalytic activity for replacing an antimony catalyst;
it is a second object of the present invention to provide a method for preparing the above titanium catalyst.
The technical scheme is as follows: the titanium catalyst comprises a compound A, wherein the compound A is in a four-membered ring or six-membered ring structure; when the compound A is in a four-membered ring structure, the structural formula is as follows:
r in the formula (1) 1 is-H or- (CH) 2 CH 3 )(CH 3 )；
When the compound A has a six-membered ring structure, the structural formula is as follows:
r in the formula (2) 2 is-CH 3 or-CH 2 CH 3 。
The preparation method of the titanium catalyst comprises the following steps: dissolving dihydroxy carboxylic acid in a solvent, slowly adding the solution into a titanium compound solution, filtering a turbid solution after the reaction is finished, and washing and drying the obtained precipitate to obtain a compound A.
Wherein the dihydroxy carboxylic acid is a compound containing two hydroxyl groups and one carboxyl group in a structural formula. When the number of carbon atoms between two hydroxyl groups of the dihydroxy carboxylic acid is 2, the obtained compound A has a four-membered ring structure; when the number of carbon atoms between two hydroxyl groups of the dihydroxy carboxylic acid is 3, the resulting compound a has a six-membered ring structure.
Further, the dihydroxy carboxylic acid is at least one of 2, 3-dihydroxypropionic acid, 2-dimethylolpropionic acid, 2-dimethylolbutyric acid, 2, 3-dihydroxy-3-methylpentanoic acid, and 3, 5-dihydroxy-3-methylpentanoic acid.
As a further preferable scheme, the titanium catalyst further comprises a compound B, the structural formula of which is as follows:
wherein the molar ratio of the compound A to the compound B is as follows: 2 is less than or equal to (A: B) is less than or equal to 6; the compound A and the compound B are physically mixed.
The preparation method of the titanium catalyst comprises the following steps:
(1) Dissolving dihydroxy carboxylic acid in a solvent, slowly adding the solution into a titanium compound solution, filtering a turbid solution after the reaction is finished, and washing and drying the obtained precipitate to obtain a compound A;
(2) Dissolving 3, 5-di-tert-butyl-4-hydroxybenzyl diethyl phosphonate in a solvent, slowly adding the solution into a titanium compound solution, filtering a turbid solution after the reaction is finished, and washing and drying the obtained precipitate to obtain a compound B;
(3) And mixing the compound A and the compound B in proportion to obtain the titanium catalyst.
Wherein the molar ratio M of the dihydroxy carboxylic acid to the titanium compound and the molar ratio M of the 3, 5-di-tert-butyl-4-hydroxybenzyl diethyl phosphonate to the titanium compound are both: 2-woven fabric (M) woven fabric (3).
Wherein, the solvent in the steps (1) and (2) is at least one of ethyl acetate, methanol, chloroform and N, N-dimethylformamide.
Wherein, the reaction conditions in the steps (1) and (2) are as follows: the reaction temperature is 55-150 ℃; the reaction time is 60-120min. The mass concentrations of the dihydroxy carboxylic acid and the 3, 5-di-tert-butyl-4-hydroxybenzyl diethyl phosphonate are respectively 10-20%, and the time for slowly adding the dihydroxy carboxylic acid and the 3, 5-di-tert-butyl-4-hydroxybenzyl diethyl phosphonate into a tetrabutyl titanate solution is respectively 30-60min;
wherein the dissolving temperature in the steps (1) and (2) is 25-150 ℃.
Wherein, the titanium compound is one of tetrabutyl titanate and tetraethyl titanate.
Wherein, in the steps (1) and (2), the drying conditions are as follows: vacuum drying oven at 60-160 deg.C for 1-3 hr.
Has the advantages that: compared with the prior art, the invention has the following remarkable effects: the titanium catalyst has the advantages of stable structure, high catalytic activity, improved product brightness, good dissolution in ethylene glycol and capability of replacing antimony catalysts; 2. the titanium catalyst of the invention has simple preparation process and is convenient for large-scale application in polyester industry.
Detailed Description
The present invention is described in further detail below.
Example 1
A preparation method of a titanium catalyst comprises the following steps:
(1) Adding 2, 2-dimethylolpropionic acid into a solvent methanol, heating to 60 ℃ to obtain a mass concentration of 20%, keeping stirring, slowly adding the mixture into a tetrabutyl titanate solution after the mixture is completely dissolved, wherein the molar ratio of the 2, 2-dimethylolpropionic acid to the tetrabutyl titanate is 2.5 after the addition is finished within 60min, and continuously stirring and reacting for 120min within the temperature range of 60 ℃ after the addition is finished. And after the reaction is finished, filtering and separating a solid product generated in the reaction process, washing the solid product for 3 times by using methanol heated to 60 ℃, and finally drying the hot-washed solid product in a vacuum oven at 80 ℃ for 2 hours to obtain a compound A1.
(2) Adding 3, 5-di-tert-butyl-4-hydroxybenzyl diethyl phosphonate into a solvent methanol, heating the obtained mass concentration to 50 ℃, keeping stirring, slowly adding the 3, 5-di-tert-butyl-4-hydroxybenzyl diethyl phosphonate into a tetrabutyl titanate solution after the 3, 5-di-tert-butyl-4-hydroxybenzyl diethyl phosphonate is completely dissolved, wherein the molar ratio of the 3, 5-di-tert-butyl-4-hydroxybenzyl diethyl phosphonate to the tetrabutyl titanate is 3 after the addition is finished within 60min, and continuously stirring and reacting for 120min within the temperature range of 60 ℃ after the addition is finished. And after the reaction is finished, filtering and separating a solid product generated in the reaction process, washing the solid product for 3 times by using methanol heated to 60 ℃, and finally drying the hot-washed solid product in a vacuum oven at 80 ℃ for 2 hours to obtain solid powder B.
(3) Mixing a compound A1 and a compound B according to a molar ratio of A1: b =2:1, and then uniformly mixing to obtain the titanium catalyst C1.
Preparation of titanium-based polyester:
adding 500g of terephthalic acid, 300g of ethylene glycol and a titanium catalyst C1 into a 2L polymerization kettle, heating to carry out esterification reaction, wherein the addition amount standard of the titanium catalyst is 5ppm based on the amount of PET titanium atoms calculated by a compound A, the temperature range of the whole esterification process is 230-250 ℃, the pressure fluctuation range during esterification is 0.2-0.3Mpa, and water produced by the reaction is discharged through a fractionating column. And (2) after esterification, releasing pressure to normal pressure, vacuumizing, heating to perform pre-polycondensation, keeping the temperature range between 250 and 280 ℃ and the pressure below 150pa for 45min, ensuring that the temperature of the prepolymer in the reaction kettle reaches 280 ℃ and the pressure reaches 150pa after pre-coalescence is finished, continuing releasing pressure, heating to perform final polycondensation, keeping the temperature range between 280 and 285 ℃ and the pressure below 100pa, stopping reaction when the system reacts to the required viscosity, extruding reactants from the bottom of the polymerization kettle by using nitrogen, cooling by water, and granulating to obtain polyester chips, wherein the test indexes are shown in table 1.
Example 2
A preparation method of a titanium catalyst comprises the following steps:
(1) Adding 2, 3-dihydroxypropionic acid into a solvent N, N-dimethylformamide to obtain a mass concentration of 15%, heating to 150 ℃, keeping stirring, slowly adding the solution into tetrabutyl titanate solution after the 2, 3-dihydroxypropionic acid is completely dissolved, and finishing the addition within 50 min; the molar ratio of the 2, 3-dihydroxypropionic acid to the tetrabutyl titanate is 2.5, and the reaction is continued to be stirred for 100min at the temperature of 150 ℃ after the addition is finished. And after the reaction is finished, filtering and separating a solid product generated in the reaction process, washing the solid product for 3 times by using N, N-dimethylformamide heated to 150 ℃, and finally drying the hot-washed solid product in a vacuum oven at 160 ℃ for 3 hours to obtain a compound A2.
(2) Mixing the compound A2 and the compound B in the example 1 in a mixing molar ratio of A2: b =3:1, and then uniformly mixing to obtain the titanium catalyst C2.
The method for preparing the titanium polyester by using the titanium catalyst C2 comprises the following steps:
the procedure was as in example 1, except that the catalyst was a titanium catalyst C2 and the test indexes of the polyester chips were as shown in Table 1.
Example 3
A preparation method of a titanium catalyst comprises the following steps:
(1) Adding 2, 3-dihydroxy-3-methyl pentanoic acid into ethyl acetate serving as a solvent, heating to 55 ℃ to obtain a mass concentration of 10%, keeping stirring, slowly adding the 3, 5-dihydroxy-3-methyl pentanoic acid into tetrabutyl titanate solution after the 3, 5-dihydroxy-3-methyl pentanoic acid is completely dissolved, wherein the molar ratio of the 3, 5-dihydroxy-3-methyl pentanoic acid to tetraethyl titanate is 2.5 after the addition is finished within 30min, and continuously stirring and reacting within the temperature range of 55 ℃ for 60min after the addition is finished. And after the reaction is finished, filtering and separating a solid product generated in the reaction process, washing the solid product for 3 times by using ethyl acetate heated to 65 ℃, and finally drying the hot-washed solid product in a vacuum oven at 80 ℃ for 3 hours to obtain a compound A3.
(2) Compound A3 was mixed with compound B in example 1 in a molar ratio of A3: b =4:1 to obtain the titanium catalyst C3 of the invention, and the test indexes of the polyester chip are shown in table 1.
The method for preparing the titanium polyester by using the titanium catalyst C3 comprises the following steps:
the procedure was as in example 1 except that the catalyst was a titanium catalyst C3.
Example 4
Compound A4 in a titanium catalyst was prepared by referring to example 1 except that the dihydroxycarboxylic acid compound was 2, 2-dimethylolbutanoic acid.
Compound A4 was mixed with compound B in example 1 at a molar ratio of A4: b =6:1, and then uniformly mixing to obtain the titanium catalyst C4.
Polyester production process reference was made to example 1, except that the catalyst was titanium catalyst C4 and the test indices for polyester chip are shown in Table 1.
Example 5
Polyester production process reference was made to example 1 except that A1 was used as catalyst, ti content was 5ppm and test criteria for polyester chips are shown in Table 1.
Example 6
Polyester production was conducted in accordance with example 2 except that A2 was used as a catalyst, ti content was 5ppm, and test indexes of the polyester chips were shown in Table 1.
Example 7
Polyester production process reference was made to example 3, except that A3 was used as catalyst, ti content 5ppm and the test indices for polyester chip are shown in Table 1.
Example 8
Polyester production process reference was made to example 4, except that A4 was used as catalyst, ti content 5ppm and the test indices for polyester chip are shown in Table 1.
Example 9
Polyester production process reference was made to example 1 except that catalyst B was used, ti content was 5ppm, and test criteria for polyester chips are shown in Table 1.
Comparative example
Polyester production process reference was made to example 1, except that ethylene glycol antimony was used as the catalyst in an amount of 200ppm, and the test indexes of the polyester chips are shown in Table 1.
TABLE 1 comparison of the Main conventional Properties of titanium-based polyesters
Claims (10)
1. A titanium catalyst comprising a compound a, wherein said compound a is a four-or six-membered ring structure; when the compound A is a four-membered ring structure, the structural formula is as follows:
r in the formula (1) 1 is-H or- (CH) 2 CH 3 )(CH 3 )；
When the compound A has a six-membered ring structure, the structural formula is as follows:
r in the formula (2) 2 is-CH 3 or-CH 2 CH 3 。
2. The titanium catalyst of claim 1, further comprising a compound B having the formula:
3. the titanium catalyst according to claim 2, characterized in that the molar ratio of compound a to compound B is: 2 is less than or equal to (A: B) is less than or equal to 6.
4. A process for preparing a titanium catalyst according to claim 1, wherein the compound A is obtained by dissolving a dihydroxycarboxylic acid in a solvent, slowly adding the solution to a solution of a titanium compound, filtering the turbid solution after the reaction is completed, and washing and drying the obtained precipitate.
5. The method for preparing a titanium catalyst according to claim 4, wherein the dihydroxy carboxylic acid is a compound having a structural formula containing two hydroxyl groups and one carboxyl group.
6. The method for preparing a titanium catalyst according to claim 4, wherein the dihydroxy carboxylic acid is at least one of 2, 3-dihydroxypropionic acid, 2-dimethylolpropionic acid, 2-dimethylolbutyric acid, 2, 3-dihydroxy-3-methylpentanoic acid, and 3, 5-dihydroxy-3-methylpentanoic acid.
7. A method for preparing the titanium catalyst according to claim 2, comprising the steps of:
(1) Dissolving dihydroxy carboxylic acid in a solvent, slowly adding the dihydroxy carboxylic acid into a titanium compound solution for reaction, filtering a turbid solution after the reaction is finished, and washing and drying the obtained precipitate to obtain a compound A;
(2) Dissolving 3, 5-di-tert-butyl-4-hydroxybenzyl diethyl phosphonate in a solvent, slowly adding the solvent into a titanium compound solution for reaction, filtering a turbid solution after the reaction is finished, and washing and drying the obtained precipitate to obtain a compound B;
(3) And mixing the compound A with the compound B to prepare the titanium catalyst.
8. The method for preparing a titanium catalyst according to claim 7, wherein the molar ratio M of the dihydroxy carboxylic acid, 3, 5-di-tert-butyl-4-hydroxybenzyldiethylphosphonate and the titanium compound is: 2-m-n-3.
9. The method for preparing a titanium catalyst according to claim 7, wherein the solvent used in the steps (1) and (2) is at least one of ethyl acetate, methanol, chloroform, and N, N-dimethylformamide.
10. The method for producing a titanium catalyst according to claim 7, wherein in the steps (1) and (2): the reaction temperature is 55-150 ℃ and the reaction time is 60-120min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116693830A (en) * | 2023-08-08 | 2023-09-05 | 富海(东营)新材料科技有限公司 | Method for preparing modified PETG copolyester by adopting quaternary ammonium titanium/zirconium chelate catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116693830A (en) * | 2023-08-08 | 2023-09-05 | 富海(东营)新材料科技有限公司 | Method for preparing modified PETG copolyester by adopting quaternary ammonium titanium/zirconium chelate catalyst |
| CN116693830B (en) * | 2023-08-08 | 2023-10-03 | 富海(东营)新材料科技有限公司 | Method for preparing modified PETG copolyester by adopting quaternary ammonium titanium/zirconium chelate catalyst |
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