Catalyst for ethylene glycol antimony and preparation process of ethylene glycol antimony

Abstract

The invention discloses a catalyst for ethylene glycol antimony and a preparation process of ethylene glycol antimony, and relates to the technical field of polyester synthesis catalysts. On one hand, the invention provides the catalyst for ethylene glycol antimony, the catalyst is cerium-loaded Uio-66-NH2 particles, and the particle size of the catalyst is 0.1-2.5 mm. On the other hand, the invention provides a preparation process of ethylene glycol antimony, antimony trichloride and ethylene glycol are mixed according to a certain proportion to serve as reaction raw materials, a small amount of catalyst for ethylene glycol antimony is added, Uio-66-NH2 particles are added to serve as an absorbent of a reaction by-product hydrogen chloride, and a pure ethylene glycol antimony product is prepared through a constant-temperature reaction. The catalyst provided by the invention can effectively improve the reaction rate of ethylene glycol antimony synthesis and the purity of the synthesized product; the ethylene glycol antimony prepared by the preparation process disclosed by the invention is relatively excellent in purity and quality and relatively low in cost.

Description

Technical Field

[0001] The present application relates to the technical field of polyester synthesis catalysts, and in particular to a catalyst for ethylene glycol antimony and a preparation process of ethylene glycol antimony. Background Art

[0002] Polyester is a general term for a class of polymers obtained by the condensation of polyacids and polyols. Commonly used thermoplastic saturated polyesters mainly include polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polybutylene terephthalate (PBT), polybutylene succinate (PBS) and their copolymers. It is a class of engineering plastics with excellent performance and wide application.

[0003] Catalysts must be used in polyester synthesis. In the history of polyester catalyst development, it has gone through a process from the initial antimony trioxide to antimony acetate, and then to ethylene glycol antimony or antimony-containing composite catalysts. Antimony catalysts have moderate catalytic speed, good product performance, and low cost. They are a very excellent polyester synthesis catalyst. Ethylene glycol antimony was introduced by Elf Chemical Company of France in the 1990s. It is a polyester synthesis catalyst that DuPont Company of the United States first realized in the direct esterification process route. Compared with antimony acetate, ethylene glycol antimony does not need to be heated and prepared; compared with antimony trioxide, it can avoid long-term heating for the catalyst to take effect; most importantly, it is an ethylene glycol compound itself, so it will not introduce impurities and can reduce the introduction of other components. Ethylene glycol antimony catalyst not only has higher solubility in ethylene glycol, high activity and high purity, but also has the advantages of good spinnability, good color and good thermal stability. Therefore, ethylene glycol antimony is far superior to antimony trioxide and antimony acetate in terms of catalytic efficiency, polymer performance and spinning effect.

[0004] The existing synthesis process of antimony glycolate is mainly based on the alcoholization process of antimony trioxide. Its synthesis route is to use antimony trioxide as the raw material, add supersaturated ethylene glycol, control a certain temperature and vacuum degree, and generate antimony glycolate by alcoholization reaction under reflux. This process requires the use of high-purity antimony trioxide and the addition of a large amount of ethylene glycol, which is relatively costly; in addition, the alcoholization reaction of this process is reversible, and the generated antimony glycolate is easily hydrolyzed, so the purity of the obtained antimony glycolate is limited. Summary of the invention

[0005] In order to solve at least one of the above technical problems, a catalyst that can effectively improve the reaction rate of ethylene glycol antimony synthesis and the purity of the synthetic product is developed, and a matching synthesis process of ethylene glycol antimony is developed. The present application provides a catalyst for ethylene glycol antimony and a preparation process of ethylene glycol antimony.

[0006] On the one hand, the present application provides a catalyst for ethylene glycol antimony, wherein the catalyst is Uio-66-NH2 particles loaded with cerium, and the particle size of the catalyst is 0.1~2.5mm.

[0007] Optionally, the particle size of the catalyst is 0.4~1mm.

[0008] On the other hand, the present application provides a process for preparing antimony ethylene glycol, comprising the following steps:

[0009] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:40-50, added into a constant temperature reactor, and the above-mentioned ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.1-0.2;

[0010] S2, adding Uio-66-NH2 particles to a constant temperature reactor according to a feed ratio of antimony trichloride to Uio-66-NH2 particles of 1:4-5;

[0011] S3, raising the temperature of the thermostatic reactor to 62-68°C, and then stirring the reaction for 60-120 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0012] S4. The reaction solution obtained in step S3 is aged for more than 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0013] Optionally, in step S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:46-48.

[0014] Optionally, in step S2, the particle size of the Uio-66-NH2 particles is 0.4~1 mm.

[0015] Optionally, in step S2, Uio-66-NH2 particles are added according to a feed ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.2~4.4.

[0016] Optionally, in step S3, the temperature of the constant temperature reactor is raised to 65-66°C.

[0017] Optionally, in step S3, the reaction is stirred for 70 to 75 minutes.

[0018] Optionally, in step S3, the filtered antimony glycol catalyst and Uio-66-NH2 particles are washed and desorbed to prepare hydrochloric acid, and the desorbed antimony glycol catalyst and Uio-66-NH2 particles are reused.

[0019] Optionally, in step S4, the aging time is 10 to 12 hours.

[0020] In summary, the present invention includes at least one of the following beneficial technical effects:

[0021] 1. The present application has discovered a catalyst that can effectively catalyze the reaction of antimony trichloride and ethylene glycol, which can effectively reduce the amount of ethylene glycol used, increase the reaction rate, and effectively improve the purity and quality of the prepared ethylene glycol antimony.

[0022] 2. This application designs a process for preparing ethylene glycol antimony. In the presence of a catalyst, antimony trichloride is used as a raw material to react with ethylene glycol to prepare ethylene glycol antimony. No other chemical reagents are introduced into the entire process, which greatly reduces the generation of impurities. The purity and quality of the obtained ethylene glycol antimony are relatively high.

[0023] 3. The preparation process of the present application uses a specially designed catalyst to catalyze the reaction, and uses Uio-66-NH2 particles as an adsorbent to adsorb the hydrogen chloride generated by the reaction. Both the catalyst and the adsorbent can be reused, and hydrochloric acid by-product can be prepared, which effectively reduces costs and improves economic benefits. In addition, the present application uses antimony trichloride as a raw material, which is much cheaper than the high-purity antimony trioxide used in existing processes, further reducing costs. DETAILED DESCRIPTION

[0024] The present application is further described in detail below with reference to the embodiments.

[0025] The present application provides a catalyst for ethylene glycol antimony, wherein the catalyst is Uio-66-NH2 particles loaded with cerium, and the particle size of the catalyst is 0.1~2.5mm.

[0026] The present application also provides a preparation process of antimony ethylene glycol, comprising the following steps:

[0027] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:40-50, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.1-0.2;

[0028] S2, adding Uio-66-NH2 particles to a constant temperature reactor according to a feed ratio of antimony trichloride to Uio-66-NH2 particles of 1:4-5;

[0029] S3, raising the temperature of the thermostatic reactor to 62-68°C, and then stirring the reaction for 60-120 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0030] S4. The reaction solution obtained in step S3 is aged for more than 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0031] In the existing technology, the synthesis process using antimony trioxide and ethylene glycol as raw materials is the mainstream industrial production process. Although some Japanese scholars have studied the synthesis process using other raw materials, none of them has the value of industrial application.

[0032] In the prior art, antimony trichloride and ethylene glycol are used as raw materials to prepare antimony glycol. However, due to the large number of side reactions, the reaction control is difficult, and the generated by-product hydrochloric acid is difficult to remove during the preparation process, which will seriously affect the preparation process. Therefore, industrial application cannot be achieved.

[0033] The present application has discovered a specific catalyst that can effectively catalyze the reaction of antimony trichloride and ethylene glycol, greatly reduce the incidence of side reactions, and adopt a specific process design to effectively remove hydrochloric acid, thereby realizing the industrial application of the synthesis process of antimony trichloride and ethylene glycol.

[0034] The following are examples of the present application.

[0035] The main raw materials used in the examples of this application are commercially available.

[0036] Among them, antimony trichloride was purchased from Shandong New Kinetic Energy Chemical Co., Ltd. with a purity of 99%; cerium-loaded Uio-66-NH2 particles and Uio-66-NH2 particles were purchased from Xi'an Qiyue Biotechnology Co., Ltd.

[0037] The following are Examples 1 to 12 of the present application.

[0038] Example 1

[0039] The preparation process of antimony ethylene glycol in this embodiment comprises the following steps:

[0040] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:40, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.1;

[0041] S2, adding Uio-66-NH2 particles to the constant temperature reactor according to the feed ratio of antimony trichloride to Uio-66-NH2 particles of 1:4;

[0042] S3, raising the temperature of the thermostatic reactor to 62°C, and then stirring the reaction for 60 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0043] S4. The reaction solution obtained in step S3 is aged for 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0044] The particle sizes of the ethylene glycol antimony catalyst and Uio-66-NH2 particles in this embodiment are both 2-2.5 mm.

[0045] Example 2

[0046] The preparation process of antimony ethylene glycol in this embodiment comprises the following steps:

[0047] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:50, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.2;

[0048] S2, adding Uio-66-NH2 particles to the constant temperature reactor according to the feed ratio of antimony trichloride to Uio-66-NH2 particles of 1:5;

[0049] S3, raising the temperature of the thermostatic reactor to 68°C, and then stirring the reaction for 120 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0050] S4. The reaction solution obtained in step S3 is aged for 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0051] The particle sizes of the ethylene glycol antimony catalyst and Uio-66-NH2 particles in this embodiment are both 2-2.5 mm.

[0052] Example 3

[0053] The preparation process of antimony ethylene glycol in this embodiment comprises the following steps:

[0054] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:46, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.15;

[0055] S2, adding Uio-66-NH2 particles to the constant temperature reactor according to the feeding ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.2;

[0056] S3, raising the temperature of the thermostatic reactor to 65°C, and then stirring the reaction for 80 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0057] S4. The reaction solution obtained in step S3 is aged for 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0058] The particle sizes of the ethylene glycol antimony catalyst and Uio-66-NH2 particles in this embodiment are both 2-2.5 mm.

[0059] Example 4

[0060] The preparation process of antimony ethylene glycol in this embodiment comprises the following steps:

[0061] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:48, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.15;

[0062] S2, adding Uio-66-NH2 particles to the constant temperature reactor according to the feeding ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.4;

[0063] S3, raising the temperature of the thermostatic reactor to 66°C, and then stirring the reaction for 80 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0064] S4. The reaction solution obtained in step S3 is aged for 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0065] The particle sizes of the ethylene glycol antimony catalyst and Uio-66-NH2 particles in this embodiment are both 2-2.5 mm.

[0066] Example 5

[0067] The preparation process of antimony ethylene glycol in this embodiment comprises the following steps:

[0068] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:46, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.15;

[0069] S2, adding Uio-66-NH2 particles to the constant temperature reactor according to the feeding ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.2;

[0070] S3, raising the temperature of the thermostatic reactor to 66°C, and then stirring the reaction for 75 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0071] S4. The reaction solution obtained in step S3 is aged for 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0072] The particle sizes of the ethylene glycol antimony catalyst and Uio-66-NH2 particles in this embodiment are both 2-2.5 mm.

[0073] Example 6

[0074] The preparation process of antimony ethylene glycol in this embodiment comprises the following steps:

[0075] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:46, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.15;

[0076] S2, adding Uio-66-NH2 particles to the constant temperature reactor according to the feeding ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.2;

[0077] S3, raising the temperature of the thermostatic reactor to 66°C, and then stirring the reaction for 70 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0078] S4. The reaction solution obtained in step S3 is aged for 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0079] The particle sizes of the ethylene glycol antimony catalyst and Uio-66-NH2 particles in this embodiment are both 2-2.5 mm.

[0080] Example 7

[0081] The preparation process of antimony ethylene glycol in this embodiment comprises the following steps:

[0082] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:45, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.12;

[0083] S2, adding Uio-66-NH2 particles to the constant temperature reactor according to the feeding ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.3;

[0084] S3, raising the temperature of the thermostatic reactor to 65°C, and then stirring the reaction for 75 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0085] S4. The reaction solution obtained in step S3 is aged for 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0086] The particle sizes of the ethylene glycol antimony catalyst and Uio-66-NH2 particles in this embodiment are both 2-2.5 mm.

[0087] Example 8

[0088] The preparation process of antimony ethylene glycol in this embodiment comprises the following steps:

[0089] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:45, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.12;

[0090] S2, adding Uio-66-NH2 particles to the constant temperature reactor according to the feeding ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.3;

[0091] S3, raising the temperature of the thermostatic reactor to 65°C, and then stirring the reaction for 75 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0092] S4. The reaction solution obtained in step S3 is aged for 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0093] The particle sizes of the ethylene glycol antimony catalyst and Uio-66-NH2 particles in this embodiment are both 0.1~0.5mm.

[0094] Example 9

[0095] The preparation process of antimony ethylene glycol in this embodiment comprises the following steps:

[0096] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:45, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.12;

[0097] S2, adding Uio-66-NH2 particles to the constant temperature reactor according to the feeding ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.3;

[0098] S3, raising the temperature of the thermostatic reactor to 65°C, and then stirring the reaction for 75 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0099] S4. The reaction solution obtained in step S3 is aged for 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0100] The particle sizes of the ethylene glycol antimony catalyst and Uio-66-NH2 particles in this embodiment are both 1.2-1.8 mm.

[0101] Example 10

[0102] The preparation process of antimony ethylene glycol in this embodiment comprises the following steps:

[0103] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:45, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.12;

[0104] S2, adding Uio-66-NH2 particles to the constant temperature reactor according to the feeding ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.3;

[0105] S3, raising the temperature of the thermostatic reactor to 65°C, and then stirring the reaction for 75 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0106] S4. The reaction solution obtained in step S3 is aged for 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0107] The particle sizes of the ethylene glycol antimony catalyst and Uio-66-NH2 particles in this embodiment are both 0.4~1mm.

[0108] Embodiment 11

[0109] The preparation process of antimony ethylene glycol in this embodiment comprises the following steps:

[0110] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:45, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.12;

[0111] S2, adding Uio-66-NH2 particles to the constant temperature reactor according to the feeding ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.3;

[0112] S3, raising the temperature of the thermostatic reactor to 65°C, and then stirring the reaction for 75 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0113] S4. The reaction solution obtained in step S3 is aged for 10 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0114] The particle sizes of the ethylene glycol antimony catalyst and Uio-66-NH2 particles in this embodiment are both 0.4~1mm.

[0115] Example 12

[0116] The preparation process of antimony ethylene glycol in this embodiment comprises the following steps:

[0117] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:45, added into a constant temperature reactor, and ethylene glycol antimony catalyst is added in a feed ratio of antimony trichloride to ethylene glycol antimony catalyst of 1:0.12;

[0118] S2, adding Uio-66-NH2 particles to the constant temperature reactor according to the feeding ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.3;

[0119] S3, raising the temperature of the thermostatic reactor to 65°C, and then stirring the reaction for 75 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles;

[0120] S4. The reaction solution obtained in step S3 is aged for 12 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0121] The particle sizes of the ethylene glycol antimony catalyst and Uio-66-NH2 particles in this embodiment are both 0.4~1mm.

[0122] Comparative Example 1

[0123] The preparation process of ethylene glycol antimony in Comparative Example 1 of the present application is different from that in Example 11 in that the catalyst for ethylene glycol antimony is replaced by an equal amount of Uio-66-NH2 particles.

[0124] Comparative Example 2

[0125] This application adopts Example 16 of the invention entitled "Method for preparing antimony glycolate" with publication number CN111635294A and invention name and "Method for preparing antimony glycolate" prepared according to the preparation method as Comparative Example 2 of this application.

[0126] Comparative Example 3

[0127] The preparation process of antimony glycolate in this comparative example comprises the following steps:

[0128] S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:54, added into a constant temperature reactor, and Uio-66-NH2 particles are added in a feed ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.8;

[0129] S2, raising the temperature of the thermostatic reactor to 70°C, and then stirring the reaction for 120 minutes, and filtering out the Uio-66-NH2 particles;

[0130] S3. The reaction solution obtained in step S3 is aged for 14 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

[0131] The particle size of the Uio-66-NH2 particles in this comparative example is 0.4~1mm.

[0132] Detection:

[0133] The ethylene glycol antimony products prepared in Examples 1 to 12 and Comparative Examples 1 to 3 of the present application were subjected to relevant performance tests, and the tests were conducted according to the method described in the industry standard YS / T 972-2014. The test results are shown in Table 1 below.

[0134] Table 1 Test results of Examples 1 to 12 and Comparative Examples 1 to 3

[0135] Antimony content (%) a value b-value L value Example 1 53.96 0.19 1.22 98.08 Example 2 57.72 0.21 1.19 98.11 Example 3 57.18 0.17 1.11 98.29 Example 4 57.04 0.19 1.14 98.26 Example 5 56.86 0.19 1.06 98.31 Example 6 56.91 0.18 1.12 98.33 Example 7 56.55 0.16 1.09 98.34 Example 8 56.26 0.14 1.02 98.37 Example 9 56.17 0.12 1.08 98.35 Example 10 56.21 0.14 1.04 98.41 Embodiment 11 55.86 0.08 0.96 98.45 Example 12 55.98 0.11 0.99 98.45 Comparative Example 1 49.7 1.94 6.08 86.62 Comparative Example 2 58.4 -0.36 1.05 98.74 Comparative Example 3 53.2 1.22 4.68 91.23

[0136] From the data in Table 1, it can be seen that the antimony content of ethylene glycol antimony prepared in Examples 1 to 12 of the present application is very close to the level of 55 to 56%, and the a value, b value and L value are all within the relevant national standards, and the L value exceeds 98%; while the quality of ethylene glycol antimony prepared in Comparative Examples 1 and 3 is greatly reduced compared with that in Examples 1 to 12 of the present application, and the quality of ethylene glycol antimony prepared in Comparative Example 2 is also slightly lower than that in Examples 1 to 12 of the present application. It can be seen that the product quality of ethylene glycol antimony prepared using the catalyst and preparation process of the present application is very excellent.

[0137] In addition, by comparing the process and test data of Examples 1 to 12 of the present application with Comparative Examples 1 and 3, it can be seen that after adding the catalyst of the present application, not only the purity and quality of the obtained antimony glycolate product have been significantly improved, but also the time consumption of the process and the amount of raw materials used have been significantly reduced. It can be seen that the catalytic effect of the catalyst of the present application is more obvious.

[0138] From the data comparison of Examples 1 to 12 in Table 1, it can be seen that after optimizing the reaction temperature and time, optimizing the raw material ratio, and optimizing the particle size of the catalyst and the absorbent, the quality of the obtained pure antimony ethylene glycol can be significantly improved.

[0139] The above are all preferred embodiments of the present application, and the protection scope of the present application is not limited thereto. Therefore, any equivalent changes made according to the structure, shape, and principle of the present application should be included in the protection scope of the present application.

Claims

1. A catalyst for antimony glycol, characterized in that: The catalyst is Uio-66-NH2 particles loaded with cerium, and the particle size of the catalyst is 0.1-2.5 mm.

2. The catalyst for antimony ethylene glycol according to claim 1, characterized in that The particle size of the catalyst is 0.4-1 mm.

3. A process for preparing antimony glycolate, characterized in that: The following steps are involved: S1. Antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:40-50, added into a constant temperature reactor, and the catalyst for antimony ethylene glycol according to any one of claims 1 or 2 is added in a feed ratio of antimony trichloride to the catalyst for antimony ethylene glycol of 1:0.1-0.2; S2, adding Uio-66-NH2 particles to a constant temperature reactor according to a feed ratio of antimony trichloride to Uio-66-NH2 particles of 1:4-5; S3, raising the temperature of the thermostatic reactor to 62-68°C, and then stirring the reaction for 60-120 minutes, filtering out the ethylene glycol antimony catalyst and Uio-66-NH2 particles; S4. The reaction solution obtained in step S3 is aged for more than 8 hours, and a solid product is obtained by suction filtration, and then vacuum drying is performed at a temperature of 90-95° C. to obtain pure antimony glycol.

4. The process for preparing antimony glycolate according to claim 3, characterized in that: In the step S1, antimony trichloride and ethylene glycol are mixed in a molar ratio of 1:46-48.

5. The process for preparing antimony glycolate according to claim 3, characterized in that: In step S2, the particle size of the Uio-66-NH2 particles is 0.4-1 mm.

6. The process for preparing antimony glycolate according to claim 3, characterized in that: In the step S2, Uio-66-NH2 particles are added according to a feed ratio of antimony trichloride to Uio-66-NH2 particles of 1:4.2-4.

4.

7. The process for preparing antimony glycolate according to claim 3, characterized in that: In step S3, the temperature of the constant temperature reactor is raised to 65-66°C.

8. The process for preparing antimony glycolate according to claim 3, characterized in that: In step S3, the reaction is stirred for 70 to 75 minutes.

9. The process for preparing antimony glycolate according to claim 3, characterized in that: In the step S3, the filtered antimony glycol catalyst and Uio-66-NH2 particles are washed and desorbed to prepare hydrochloric acid, and the desorbed antimony glycol catalyst and Uio-66-NH2 particles are reused.

10. The process for preparing antimony glycolate according to claim 3, characterized in that: In step S4, the aging time is 10 to 12 hours.