CN1235148A - Preparation of high purity antimony glycol - Google Patents
Preparation of high purity antimony glycol Download PDFInfo
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- CN1235148A CN1235148A CN 99114156 CN99114156A CN1235148A CN 1235148 A CN1235148 A CN 1235148A CN 99114156 CN99114156 CN 99114156 CN 99114156 A CN99114156 A CN 99114156A CN 1235148 A CN1235148 A CN 1235148A
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- purity antimony
- antimony
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Abstract
A process for preparing high-purity glycol antimony as catalyst includes esterifying-dewatering reaction of excess glycol Sb2O3 at 120-180 deg.C, filtering, cooling crystallization, recrystallization with glycol, washing with alcohol to remove glycol and drying. It is superior to antimony acetate and Sb2O3 in performance. Its advantages include high solubility in glycol, purity and catalytic activity. If it is used in granulation of polyester, good colour and high spinning output rate are resulted in.
Description
The present invention relates to a kind of catalyzer that is used for the polyethylene terephthalate polycondensation, especially a kind of preparation method of high purity antimony glycol.
The catalyzer that is used for polyethylene terephthalate and Poly(Trimethylene Terephthalate) polycondensation, commonly used has the titaniferous inorganic ester as catalyzer, stibiated catalyzer also has reported in literature, as traditional polyester catalyst antimony acetate, antimonous oxide is arranged, and they cut both ways on using.As activity antimony acetate preferably, it is low and in application process equipment is had corrosion to contain the antimony amount; Contain the higher antimonous oxide of antimony amount and be insoluble in ethylene glycol, influence activity of such catalysts again.The chemical molecular formula of antimony glycol is: Sb
2(OCH-CHO)
3, the main application of antimony glycol is the catalyzer as the polycondensation of terephthalate.Its solubleness in ethylene glycol solution is big, and the content of antimony is the highest in the soluble antimony catalyzer, and is not mixed with any impurity, the purity height, the polycondensate of terephthalate (being polyester) has the favorable extensibility energy when the spray silk, be difficult for fracture of wire, the polyester product color and luster is better.
The objective of the invention is: preparation is better than catalyzer--the antimony glycol of antimony acetate and antimonous oxide, and it has the advantages that solubleness is good in ethylene glycol, purity is high, catalytic activity is high, makes its polyester granulation color and luster good, spray silk productive rate height.
The object of the present invention is achieved like this: a kind of preparation method of high purity antimony glycol, it is characterized in that excessive ethylene glycol and antimonous oxide carry out the esterification dehydration reaction in 120-180 ℃ temperature range, crystallisation by cooling after filtration,, and the spent glycol recrystallization, remove ethylene glycol and carry out drying with the alcohol washing.
Further improvement of the present invention is to carry out esterification with excessive ethylene glycol and antimonous oxide, and its mol ratio is 1: 3-50.In addition, in esterification, feed shielding gas, generally use nitrogen.
Characteristics of the present invention are: the high purity antimony glycol of gained is better than antimony acetate and antimonous oxide catalyzer.Have the advantages that solubleness is good in ethylene glycol, purity is high, catalytic activity is high, make the color and luster of polyester granulation good, spray silk productive rate height.
The invention will be further described below in conjunction with embodiment:
The high purity antimony glycol preparation, in 120-180 ℃ temperature range, carry out the esterification dehydration reaction with excessive ethylene glycol and antimonous oxide, after filtration, crystallisation by cooling, and spent glycol recrystallization is removed ethylene glycol and carry out drying under reduced pressure with the alcohol washing.The alcohols of washing is a low-carbon alcohol, generally is anhydrous methanol and ethanol, and the ethylene glycol that crystallisate is is cleaned.
Example 1. antimonous oxides 291.5 grams, 260 kilograms of ethylene glycol are heated to 165-180 ℃, feed nitrogen.Wait distillates water when reaching 53.5 grams (theoretical aquifer yield 54 gram), stops heating, heat filtering.Crystallisation by cooling filters filter flask spent glycol recrystallization, crystallisate absolute ethanol washing.This crystallisate carries out drying under reduced pressure, obtain even fine particle crystallization antimony glycol.
Experimental result as:
(1) ultimate analysis:
Experimental data Theoretical Calculation number
C 16.96％ 17.10％
H 3.14％ 2.86％
Sb 57.50％ 57.48％
The chemical molecular formula of the water yield susceptible of proof antimony glycol that generates according to the ultimate analysis data and in preparation process is: Sb
2(OCH-CHO)
3
(2) product analysis
Antimony content 57.50%
Iron level does not detect
Chloride ion content＜0.005%
Sulfate radical content＜0.01%
Example 2. antimonous oxides 50 grams, ethylene glycol 460 grams are heated to 150-160 ℃, feed nitrogen, and water to be distillated reaches 9 grams (theoretical water outlet one 9.26 grams), stops heating, heat filtering.Crystallisation by cooling filters, and filter flask spent glycol recrystallization, crystallisate anhydrous methanol repetitive scrubbing, this crystallisate obtain even fine particle crystallization antimony glycol in the descending drying of reduced pressure.Experimental result is with example 3.
Example 3. antimonous oxides 30 grams, ethylene glycol 1000 grams are heated to 130-140 ℃, feed nitrogen, and water to be distillated reaches 6 grams, stops heating, heat filtering.Crystallisation by cooling filters, and filter flask spent glycol recrystallization, crystallisate anhydrous methanol repetitive scrubbing, this crystallisate obtain even fine particle crystallization antimony glycol in the descending drying of reduced pressure.
Experimental result as:
(1) ultimate analysis:
Experimental data Theoretical Calculation number
C 16.97％ 17.10％
H 3.16％ 2.86％
Sb 57.10％ 57.48％
(2) product analysis:
Antimony content 57.60%
Iron level 0.0004%
Chloride ion content＜0.005%
Sulfate ion content＜0.01%
Example 4. antimonous oxides 290 grams, ethylene glycol 210 grams are heated to 170-180 ℃, feed argon gas, with other processing condition of example 3, obtain even fine particle crystallization antimony glycol.
Example 5. antimonous oxides 250 grams, ethylene glycol 800 grams are heated to 130-140 ℃, obstructed shielding gas, with other condition of example 1, general gas drying obtains even fine particle crystallization antimony glycol.
The analytical results of example 4,5 is example 1 roughly the same.
Claims (6)
1. the preparation method of a high purity antimony glycol, it is characterized in that excessive ethylene glycol and antimonous oxide carry out the esterification dehydration reaction in 120-180 ℃ temperature range, after filtration, crystallisation by cooling, and spent glycol recrystallization is removed ethylene glycol and is carried out drying with the alcohol washing.
2. by the preparation method of the described high purity antimony glycol of claim 1, it is characterized in that carrying out esterification with excessive ethylene glycol and antimonous oxide, its mol ratio is 1: 3-50.
3. by the preparation method of the described high purity antimony glycol of claim 1, it is characterized in that in esterification, feeding shielding gas.
4. by the preparation method of the described high purity antimony glycol of claim 3, it is characterized in that with nitrogen as shielding gas.
5. by the preparation method of the described high purity antimony glycol of claim 1, it is characterized in that temperature of reaction is heated to 165-180 ℃, feed nitrogen.
6. by the preparation method of the described high purity antimony glycol of claim 1, it is characterized in that dry air carries out drying under reduced pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99114156 CN1235148A (en) | 1999-04-16 | 1999-04-16 | Preparation of high purity antimony glycol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99114156 CN1235148A (en) | 1999-04-16 | 1999-04-16 | Preparation of high purity antimony glycol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1235148A true CN1235148A (en) | 1999-11-17 |
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Family Applications (1)
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|---|---|---|---|
| CN 99114156 Pending CN1235148A (en) | 1999-04-16 | 1999-04-16 | Preparation of high purity antimony glycol |
Country Status (1)
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| CN (1) | CN1235148A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1075510C (en) * | 1999-10-26 | 2001-11-28 | 郑立梅 | Glycol antimony catalyst and preparation process thereof |
| CN1112340C (en) * | 2000-01-12 | 2003-06-25 | 曹善文 | Process for preparing antimony compound of binary alcohol |
| CN100355713C (en) * | 2002-03-29 | 2007-12-19 | 北京石油化工学院 | Prepn of glycol antimony |
| CN1891708B (en) * | 2005-07-05 | 2010-04-14 | 李绍通 | Process for synthesizing organometallic antimonide |
| CN101735013A (en) * | 2008-11-19 | 2010-06-16 | 辽阳市宏伟区合成催化剂厂 | Process for preparing ethylene glycol antimony serving as polyester polycondensation catalyst |
| CN102866909A (en) * | 2012-08-27 | 2013-01-09 | 北京奇虎科技有限公司 | Resource lock system and method for controlling interface resource access |
| CN103435793A (en) * | 2013-09-10 | 2013-12-11 | 杭州金海湾化工有限公司 | Polyester catalyst, and preparation method and application thereof |
| CN103435786A (en) * | 2013-09-10 | 2013-12-11 | 杭州金海湾化工有限公司 | Liquid polyester catalyst, and preparation method and application thereof |
| CN111635294A (en) * | 2020-06-08 | 2020-09-08 | 金浦新材料股份有限公司 | Method for preparing ethylene glycol antimony and ethylene glycol antimony prepared according to method |
-
1999
- 1999-04-16 CN CN 99114156 patent/CN1235148A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1075510C (en) * | 1999-10-26 | 2001-11-28 | 郑立梅 | Glycol antimony catalyst and preparation process thereof |
| CN1112340C (en) * | 2000-01-12 | 2003-06-25 | 曹善文 | Process for preparing antimony compound of binary alcohol |
| CN100355713C (en) * | 2002-03-29 | 2007-12-19 | 北京石油化工学院 | Prepn of glycol antimony |
| CN1891708B (en) * | 2005-07-05 | 2010-04-14 | 李绍通 | Process for synthesizing organometallic antimonide |
| CN101735013A (en) * | 2008-11-19 | 2010-06-16 | 辽阳市宏伟区合成催化剂厂 | Process for preparing ethylene glycol antimony serving as polyester polycondensation catalyst |
| CN102866909A (en) * | 2012-08-27 | 2013-01-09 | 北京奇虎科技有限公司 | Resource lock system and method for controlling interface resource access |
| CN103435793A (en) * | 2013-09-10 | 2013-12-11 | 杭州金海湾化工有限公司 | Polyester catalyst, and preparation method and application thereof |
| CN103435786A (en) * | 2013-09-10 | 2013-12-11 | 杭州金海湾化工有限公司 | Liquid polyester catalyst, and preparation method and application thereof |
| CN103435793B (en) * | 2013-09-10 | 2015-09-02 | 杭州金海湾化工有限公司 | A kind of polyester catalyst and its preparation method and application |
| CN103435786B (en) * | 2013-09-10 | 2016-01-13 | 杭州金海湾化工有限公司 | A kind of liquid polyesters Catalysts and its preparation method and application |
| CN111635294A (en) * | 2020-06-08 | 2020-09-08 | 金浦新材料股份有限公司 | Method for preparing ethylene glycol antimony and ethylene glycol antimony prepared according to method |
| CN111635294B (en) * | 2020-06-08 | 2022-08-16 | 金浦新材料股份有限公司 | Preparation method of ethylene glycol antimony and ethylene glycol antimony prepared according to preparation method |
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