CN102432567A - Method for preparing epoxy succinate - Google Patents
Method for preparing epoxy succinate Download PDFInfo
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- CN102432567A CN102432567A CN2011103471718A CN201110347171A CN102432567A CN 102432567 A CN102432567 A CN 102432567A CN 2011103471718 A CN2011103471718 A CN 2011103471718A CN 201110347171 A CN201110347171 A CN 201110347171A CN 102432567 A CN102432567 A CN 102432567A
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- maleic anhydride
- sodium
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Abstract
The invention relates to a method for preparing epoxy succinate, which comprises the following steps of: producing a maleic acid disodium salt by using sodium carbonate or sodium bicarbonate, water and maleic anhydride as raw materials; and under the condition of using sodium tungstate as a catalyst, synthetizing the epoxy succinate by using hydrogen peroxide as the raw material. Due to the adoption of sodium carbonate or sodium bicarbonate which is used as the raw material, the reaction process is more mild and controllable, a system is more stable to operate, the raw materials are relatively cheap, a small quantity of water is produced in the reaction process, the epoxy succinate has high solid content, and the quality of the epoxy succinate is easier to control.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of preparation method of epoxy succinic hydrochlorate.
Background technology
The epoxy succinic hydrochlorate is a kind of important chemical material, also is the midbody of poly-epoxy succinic acid building-up process.In the research of poly-epoxy succinic acid; Part about the synthesizing epoxy SUMATRIPTAN SUCCINATE; More representational have a U.S. Pat 4654159, and its operational path is that MALEIC ANHYDRIDE is dissolved in the water, adds sodium hydroxide again and generate maleic acid sodium, and the adding sodium wolframate is catalyzer, adds hydrogen peroxide continuously; Regulate and maintenance reaction process pH=5～7 synthesizing epoxy succsinic acid sodium salt with sodium hydroxide.In the claim of domestic related patent U.S. Patent No. CN1470493A; Propose to adopt the MALEIC ANHYDRIDE generation maleic acid that is dissolved in the water; Add aqueous sodium hydroxide solution until pH=5～7; Add a certain amount of sodium tungstate catalyst, under 50～100 ℃ of temperature, add aqueous hydrogen peroxide solution synthesizing epoxy succsinic acid sodium salt continuously.Domestic patent CN101538362A proposes maleic anhydride is used deionized water dissolving, and 30 ℃～60 ℃ stirrings add sodium hydroxide solution down, and controlled temperature adds sodium wolframate, hydrogen peroxide down for 60 ℃～100 ℃; Regulate pH=5～7; Reacted 2～100 hours, and be cooled to then below 20 ℃, add a kind of precipitant mix and stir; Add water behind the suction filtration, keep pH and be heated to 70 ℃～100 ℃ 6～7 and obtain Epoxysuccinic acid.
In the above-mentioned epoxy succinic hydrochlorate synthesis technique, adopt sodium hydroxide as raw material usually, sodium hydroxide belongs to strongly alkaline compound; Neutralization reaction takes place when mixing with the acidic cpd MALEIC ANHYDRIDE; Generate a large amount of reaction heat, reaction process is violent, temperature control difficulty in the reaction process.Simultaneously, sodium hydroxide is as the main industrial chemicals of this technology, and its price is higher relatively, and the production cost of epoxy succinic hydrochlorate is had considerable influence.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of epoxy succinic hydrochlorate; Its characteristic comprises: with yellow soda ash or sodium hydrogencarbonate, water, MALEIC ANHYDRIDE is that raw material generates maleic acid disodium salt salt; At sodium wolframate is under the condition of catalyzer, is raw material synthesizing epoxy SUMATRIPTAN SUCCINATE with the hydrogen peroxide.This method adopts yellow soda ash or sodium hydrogencarbonate as raw material, replacing sodium hydroxide raw material commonly used at present, under the constant basically situation of other reaction conditions, can obtain the epoxy succinic acid salt solution of better quality.Its main technique step is:
Fs: the mol ratio by MALEIC ANHYDRIDE and water is 1: (5～10); MALEIC ANHYDRIDE is dissolved; Add carbonic acid (hydrogen) sodium raw materials; Generate maleic acid disodium salt salt, the mol ratio of control yellow soda ash and MALEIC ANHYDRIDE is (3～5): 4, and the mol ratio of sodium hydrogencarbonate and MALEIC ANHYDRIDE is (2～4): 2;
Subordinate phase: press 0.1%～10% of maleic acid mole number and add sodium wolframate; Under 50～70 ℃, add the hydrogen peroxide raw material continuously, total add-on of hydrogen peroxide is 1.0～1.2 times of MALEIC ANHYDRIDE mole number; Joining day≤30min; Use carbonic acid (hydrogen) sodium control pH=5～7 simultaneously, 30min～6h under 60～80 ℃ of conditions of constant temperature generates the epoxy succinic hydrochlorate.
In the methods of the invention, comprise that employing adds corresponding MALEIC ANHYDRIDE and water in carbonic acid (hydrogen) sodium solution, to realize the fs reaction.
Beneficial effect of the present invention is: in synthesizing epoxy SUMATRIPTAN SUCCINATE process, use weakly alkaline raw material carbonic acid (hydrogen) sodium to replace alkaline industrial raw material sodium hydroxide solution, the reaction process gentleness is controlled; System's operation is more stable; Raw material is relatively cheap, and in the reaction process, the water yield of generation is few; The product solid content is higher, and product quality is controlled more easily.
Embodiment
Embodiment 1
In the 500mL four-hole bottle of whisking appliance, reflux exchanger is housed, add 49g (0.5 mole) MALEIC ANHYDRIDE, 100ml water, under agitation slowly add about 35gNa
2CO
3Solid.With the temperature of the water-bath hierarchy of control below 55 ℃.Add aqueous hydrogen peroxide solution continuously with volume pump, 68g hydrogen peroxide (30% aqueous solution) is added in 30min, keep pH=6～6.5,60 ℃ constant temperature 1.5h with yellow soda ash control pH simultaneously, obtain epoxy sodium succinate.Through the chromatography of ions test, Epoxysuccinic acid purity reaches 91.64%.
Embodiment 2
In the 500mL four-hole bottle of whisking appliance, reflux exchanger is housed, add 49g (0.5 mole) MALEIC ANHYDRIDE, 100ml water, under agitation slowly add about 45gNa
2CO
3Solid.With the temperature of the water-bath hierarchy of control below 55 ℃.Add aqueous hydrogen peroxide solution continuously with volume pump, 68g hydrogen peroxide (30% aqueous solution) is added in 30min, control pH=6.5～7,65 ℃ constant temperature 1.5h with yellow soda ash simultaneously, obtain epoxy sodium succinate.Through the chromatography of ions test, Epoxysuccinic acid purity reaches 92.60%.
Embodiment 3
In the 500mL four-hole bottle of whisking appliance, reflux exchanger is housed, add 49g (0.5 mole) MALEIC ANHYDRIDE, 100g water, under agitation slowly add about 60gNaHCO
3Solid.With the temperature of the water-bath hierarchy of control below 55 ℃.Use 68g hydrogen peroxide (30% aqueous solution) is added in 30min, use NaHCO simultaneously
3Control pH=6～6.5,60 ℃ constant temperature 1.5h obtains epoxy sodium succinate.Through test, Epoxysuccinic acid purity reaches 90.60%.
Embodiment 4
In the 500mL four-hole bottle of whisking appliance, reflux exchanger is housed, add 49g (0.5 mole) MALEIC ANHYDRIDE, 100g water, under agitation slowly add about 70gNaHCO
3Solid.With the temperature of the water-bath hierarchy of control below 55 ℃.Use 68g hydrogen peroxide (30% aqueous solution) is added in 30min, use NaHCO simultaneously
3Control pH=6.5～7,65 ℃ constant temperature 1.5h obtains epoxy sodium succinate.Through test, Epoxysuccinic acid purity reaches 91.80%.
Claims (2)
1. the preparation method of an epoxy succinic hydrochlorate, this method is that raw material generates maleic acid disodium salt salt with yellow soda ash or sodium hydrogencarbonate, water, MALEIC ANHYDRIDE, is under the condition of catalyzer at sodium wolframate, is raw material synthesizing epoxy SUMATRIPTAN SUCCINATE with the hydrogen peroxide.Its concrete steps have:
Fs: the mol ratio by MALEIC ANHYDRIDE and water is 1: (5～10); MALEIC ANHYDRIDE is dissolved; Add carbonic acid (hydrogen) sodium raw materials; Generate maleic acid disodium salt salt, the mol ratio of control yellow soda ash and MALEIC ANHYDRIDE is (3～5): 4, and the mol ratio of sodium hydrogencarbonate and MALEIC ANHYDRIDE is (2～4): 2;
Subordinate phase: press 0.1%～10% of MALEIC ANHYDRIDE mole number and add sodium wolframate; Under 50～70 ℃, add the hydrogen peroxide raw material continuously, total add-on of hydrogen peroxide is 1.0～1.2 times of MALEIC ANHYDRIDE mole number; Joining day≤30min; Use carbonic acid (hydrogen) sodium control pH=5～7 simultaneously, 30min～6h under 60～80 ℃ of conditions of constant temperature generates the epoxy succinic hydrochlorate.
2. the preparation method of epoxy succinic hydrochlorate according to claim 1 is characterized in that MALEIC ANHYDRIDE and water are added in carbonic acid (hydrogen) sodium solution, obtains maleic acid disodium salt salt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110347171.8A CN102432567B (en) | 2011-11-07 | 2011-11-07 | Method for preparing epoxy succinate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110347171.8A CN102432567B (en) | 2011-11-07 | 2011-11-07 | Method for preparing epoxy succinate |
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| CN102432567A true CN102432567A (en) | 2012-05-02 |
| CN102432567B CN102432567B (en) | 2015-01-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709387A (en) * | 2013-12-19 | 2014-04-09 | 南宁市化工研究设计院 | Production method of polyepoxysuccinic acid |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4654159A (en) * | 1985-06-24 | 1987-03-31 | The Procter & Gamble Company | Ether hydroxypolycarboxylate detergency builders |
| CN1524893A (en) * | 2003-02-28 | 2004-09-01 | 赵勇军 | Synthesis of poly epoxy succinate |
| CN1683313A (en) * | 2004-12-09 | 2005-10-19 | 兰州理工大学 | Epoxy sodium succinate and its process for preparing polymer |
| CN101602852A (en) * | 2009-07-13 | 2009-12-16 | 山东省泰和水处理有限公司 | A kind of preparation method of polyepoxy sodium succinate for water treatment |
| CN101717498A (en) * | 2009-12-16 | 2010-06-02 | 内蒙古天晨科技有限责任公司 | Synthesis method of high-concentration polyepoxysuccinic acid and salt thereof |
-
2011
- 2011-11-07 CN CN201110347171.8A patent/CN102432567B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4654159A (en) * | 1985-06-24 | 1987-03-31 | The Procter & Gamble Company | Ether hydroxypolycarboxylate detergency builders |
| CN1524893A (en) * | 2003-02-28 | 2004-09-01 | 赵勇军 | Synthesis of poly epoxy succinate |
| CN1683313A (en) * | 2004-12-09 | 2005-10-19 | 兰州理工大学 | Epoxy sodium succinate and its process for preparing polymer |
| CN101602852A (en) * | 2009-07-13 | 2009-12-16 | 山东省泰和水处理有限公司 | A kind of preparation method of polyepoxy sodium succinate for water treatment |
| CN101717498A (en) * | 2009-12-16 | 2010-06-02 | 内蒙古天晨科技有限责任公司 | Synthesis method of high-concentration polyepoxysuccinic acid and salt thereof |
Non-Patent Citations (3)
| Title |
|---|
| 吕志芳: "环氧琥珀酸的合成条件研究", 《精细石油化工》, no. 3, 31 May 2001 (2001-05-31) * |
| 杨燕，等: "采用复合催化剂合成环氧琥珀酸", 《石油天然气学报(江汉石油学院学报)》, vol. 32, no. 1, 28 February 2010 (2010-02-28) * |
| 梁宝锋，等: "环氧琥珀酸及其聚合物的合成研究", 《石化技术与应用》, vol. 26, no. 1, 31 January 2008 (2008-01-31) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709387A (en) * | 2013-12-19 | 2014-04-09 | 南宁市化工研究设计院 | Production method of polyepoxysuccinic acid |
| CN103709387B (en) * | 2013-12-19 | 2016-04-27 | 南宁市化工研究设计院 | Production method of polyepoxysuccinic acid |
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| CN102432567B (en) | 2015-01-07 |
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