Ethylene glycol antimony as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of chemical engineering, and particularly relates to ethylene glycol antimony and a preparation method and application thereof.The preparation method comprises the steps that firstly, antimonous oxide and ethylene glycol with the mass ratio being 1: (8-10) are added into a preheating reaction kettle, steam heating is conducted for 1-1.5 h at the temperature of 130 DEG C, pulping is conducted, then slurry is conveyed to a main reaction kettle, a vacuumizing electric heating reaction is conducted, and a reaction product is obtained; the electric heating temperature is 450-460 DEG C, and the reaction time is 5-6 hours, filtering until the solution is transparent, conveying to a crystallization kettle, crystallizing, centrifuging, washing and drying to obtain ethylene glycol antimony; the problem that in the prior art, due to the fact that antimony trioxide and ethylene glycol are subjected to reversible reaction, the dissolution transmittance of ethylene glycol antimony is low due to the fact that the temperature is too high or too low is solved, and the problem that in the prior art, due to the fact that antimony trioxide and ethylene glycol are subjected to reversible reaction, the dissolution transmittance of ethylene glycol antimony needs to be guaranteed due to excessive raw materials is solved.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical industry, and specifically relates to antimony glycol and a preparation method and application thereof. Background Art

[0002] Antimony glycolate is a white crystalline powder that is easily soluble in ethylene glycol and decomposes easily when exposed to moisture. It is a novel catalyst used in polyester polycondensation reactions.

[0003] The prior art generally adopts two methods: (1) using metal antimony as a sacrificial anode, an inert material as a cathode, and an ethylene glycol solution containing an electrolyte as an electrolyte, and passing direct current for electrolysis in a single-chamber electrolytic cell, reducing at the cathode to obtain black active antimony, and the active antimony reacts with ethylene glycol, and after separation, washing and drying, an ethylene glycol antimony product is obtained. The raw materials used in this preparation process are not easy and the energy consumption is large; (2) using antimony trioxide and ethylene glycol (molar ratio = 1:40-50) to react at 170-180°C and vacuum conditions for 150 minutes. This reaction is a reversible reaction, which requires an excess of raw materials and is costly. In addition, this method has a high reaction temperature and a long reaction time, which will increase the number of by-products and reduce the color and quality of the product. Summary of the invention

[0004] The purpose of the present invention is to solve the deficiencies in the prior art and to provide antimony glycol and a preparation method and application thereof.

[0005] In order to achieve the above object, the present invention is achieved through the following technical solutions:

[0006] In a first aspect, the present invention provides a method for preparing antimony ethylene glycol, the method comprising the following steps:

[0007] (1) Add antimony trioxide and ethylene glycol in a mass ratio of 1:8-10 into a preheated reactor, and steam heat at 130°C for 1-1.5 hours to perform pulping.

[0008] (2) The slurry is then transferred to the main reactor for vacuum electric heating reaction at a temperature of 450-460°C for 5-6 hours until the solution becomes transparent, filtered, and transferred to a crystallization kettle for crystallization.

[0009] (3) Centrifuge, wash and dry to obtain antimony ethylene glycol.

[0010] Preferably, in step (1), the order of adding antimony trioxide and ethylene glycol into the preheating reactor is to add ethylene glycol first and then add antimony trioxide.

[0011] Preferably, in step (2), the crystallization reaction speed is controlled to be 10-80 rpm.

[0012] Preferably, ethanol is used for washing in step (3).

[0013] Preferably, the drying conditions in step (3) are: heating and drying in a vacuum water bath at 95°C and -0.07Mpa.

[0014] In a second aspect, the present invention provides ethylene glycol antimony, which is prepared by the above method.

[0015] In a third aspect, the present invention provides an application of the ethylene glycol antimony, wherein the ethylene glycol antimony is applied as a polyester polycondensation catalyst.

[0016] The present invention has the following beneficial effects: (1) The present invention preheats the low-temperature reaction and then conducts the high-temperature heating reaction in the main reactor, thereby solving the problem in the prior art that the antimony trioxide and ethylene glycol are reversible reactions and that excessively high or low temperatures will result in low dissolution permeability of ethylene glycol antimony. The present invention solves the problem in the prior art that the antimony trioxide and ethylene glycol are reversible reactions and that excessive amounts of raw materials are required to ensure the dissolution permeability of ethylene glycol antimony.

[0017] (2) In the first step of the reaction, the present invention uses low-temperature steam heating for pre-reaction, and then performs high-temperature heating to generate a temperature gradient, accelerate the esterification rate, facilitate the formation of ethylene glycol antimony, and reduce by-products.

[0018] (3) The present invention adopts vacuum water bath heating drying to further reduce the drying loss. DETAILED DESCRIPTION

[0019] The present invention will be further described below in conjunction with the embodiments, but they are not intended to limit the present invention.

[0020] Example 1

[0021] In the preheating reactor, 3600 kg of ethylene glycol and 450 kg of antimony trioxide were added in sequence, and steam-heated at 130°C for 1 hour for slurrying. The slurry was then transported to the main reactor through a pipeline for vacuum electric heating at 450°C. The reaction was carried out for 5 hours until the solution became transparent, and then filtered. The solution was transported to a crystallization kettle through a pipeline for crystallization at a rotation speed of 40 rpm, and then centrifuged, washed with ethanol, and dried to obtain ethylene glycol antimony.

[0022] Example 2

[0023] In the preheating reactor, 4500kg of ethylene glycol and 500kg of antimony trioxide were added in sequence, and steam-heated at 130°C for 1.2h for slurrying. Then the slurry was transported to the main reactor through a pipeline for vacuum electric heating at a temperature of 455°C. The reaction was carried out for 5.5h until the solution became transparent, then filtered, and transported to a crystallization kettle through a pipeline for crystallization at a rotation speed of 60rmp. After that, it was centrifuged, washed with ethanol, and dried to obtain ethylene glycol antimony.

[0024] Example 3

[0025] In the preheating reactor, 5500 kg of ethylene glycol and 550 kg of antimony trioxide were added in sequence, and steam-heated at 130°C for 1.5 hours for slurrying. The slurry was then transported to the main reactor through a pipeline for vacuum electric heating at 460°C. The reaction was carried out for 6 hours until the solution became transparent, then filtered, and transported to a crystallization kettle through a pipeline for crystallization at a rotation speed of 80 rpm. The mixture was then centrifuged, washed with ethanol, and dried to obtain ethylene glycol antimony.

[0026] Example 4

[0027] Add 5500kg of ethylene glycol and 550kg of antimony trioxide into the preheating reactor in sequence, steam heat at 130°C for 1.5h, slurry, and then transport the slurry to the main reactor through a pipeline for vacuum electric heating at 460°C. React for 6h until the solution is transparent, filter, and transport to a crystallization kettle through a pipeline for crystallization at a speed of 80rmp. Then centrifuge, wash with ethanol, and dry under -0.07Mpa, 95°C water bath heating and drying conditions to obtain ethylene glycol antimony.

[0028] Comparative Example 1

[0029] Antimony trioxide and ethylene glycol were added in a molar ratio of 1:50, and ethylene glycol antimony was obtained under vacuum conditions at a reaction temperature of 170° C. and a reaction time of 150 min.

[0030] Comparative Example 2

[0031] Antimony trioxide and ethylene glycol were added in a molar ratio of 1:40, and ethylene glycol antimony was obtained under vacuum conditions with a reaction temperature of 175° C. and a reaction time of 160 min.

[0032] Comparative Example 3

[0033] Antimony trioxide and ethylene glycol were added in a molar ratio of 1:50, and ethylene glycol antimony was obtained under vacuum and steam heating conditions with a reaction temperature of 170° C. and a reaction time of 150 min.

[0034] The quality of the antimony ethylene glycol products obtained in Examples 1-4 and Comparative Examples 1-3 was tested, and the results are shown in Table 1.

[0035] Table 1 Comparison of the quality of the products of the embodiments and comparative examples

[0036]

[0037] As can be seen from Table 1, Comparative Examples 1 and 2 only undergo heating reaction, and the dissolution permeability of ethylene glycol antimony is low, the L value is low, the antimony content is low, and the iron and lead contents are high. Comparative Example 3 adopts steam heating relative to Comparative Examples 1 and 2, and the dissolution permeability of ethylene glycol antimony is improved, but it is lower than that of Example 3. Example 1-3 undergoes low-temperature reaction in a preheating reactor and then undergoes high-temperature heating reaction in a main reactor, which improves the dissolution permeability of ethylene glycol antimony, has a high L value, high antimony content, low iron and lead contents, and the drying loss meets the standard. As can be seen from Example 4, the use of vacuum water bath heating drying can reduce the drying loss and is closer to the standard.

[0038] The above shows and describes the basic principles, main features and advantages of the present invention. However, the above is only a specific embodiment of the present invention, and the technical features of the present invention are not limited thereto. Any other implementation methods derived by any technician in the field without departing from the technical solution of the present invention should be included in the patent scope of the present invention.

Claims

1. A method for preparing antimony glycolate, characterized in that: The method comprises the following steps: (1) Add antimony trioxide and ethylene glycol in a mass ratio of 1:8-10 into a preheated reactor, and steam heat at 130°C for 1-1.5 hours to perform pulping. (2) The slurry is then transferred to the main reactor for vacuum electric heating reaction at a temperature of 450-460°C for 5-6 hours until the solution becomes transparent, filtered, and transferred to a crystallization kettle for crystallization. (3) Centrifuge, wash and dry to obtain antimony ethylene glycol.

2. The method for preparing antimony glycolate according to claim 1, characterized in that: In step (1), the order of adding antimony trioxide and ethylene glycol to the preheating reactor is to add ethylene glycol first and then add antimony trioxide.

3. The method for preparing antimony glycolate according to claim 1, characterized in that: In step (2), the crystallization reaction speed is controlled to be 10-80 rpm.

4. The method for preparing antimony glycolate according to claim 1, characterized in that: In step (3), ethanol is used for washing.

5. The method for preparing antimony glycolate according to claim 1, characterized in that: The drying conditions in step (3) are: heating and drying in a vacuum water bath at 95°C and -0.07Mpa.

6. Antimony glycolate, characterized in that: The antimony ethylene glycol is prepared by the method according to any one of claims 1 to 5.

7. An application of antimony glycolate according to claim 6, characterized in that: The antimony glycol is applied to polyester polycondensation catalyst.

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