Method for synthesizing polyepoxysuecinic acid salt

A technology of polyepoxysuccinate and epoxysuccinate, applied in the field of synthesis of polyepoxysuccinate, can solve the problems of low quality synthetic PESA, many by-products, large amount of acetone, etc. It is beneficial to the polymerization reaction, overcomes the low degree of polymerization, and inhibits the effect of hydrolysis.

Inactive Publication Date: 2011-11-09
北京合创同盛科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The main problem occurring in the prior art is that there are many by-products in the one-step reaction system, and the Ca(OH) as initiator 2 Large dosage, poor repeatability
The quality of synthetic PESA is not high, and the effective content of PESA is low, which affects the use effect as a scale inhibitor
However, the price of raw materials in the multi-step method is high, the amount of acetone is large, and the cost of synthesizing PESA is high.
Considering the economical use of scale inhibitors in the current market, it is not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 49 grams of maleic anhydride (Fushun Petrochemical Company) into a four-necked flask, add 80ml of deionized water to dissolve, slowly add 60 grams of 50% NaOH solution under stirring at 50°C, then heat to 75°C on a water bath, and add tungstic acid Sodium (Nantong Wanbang Technology Fine Chemical Co., Ltd.) 1.7 g, slowly add 65 ml of 30% hydrogen peroxide (Beijing Xunda Chemical & Hardware Co., Ltd.), dropwise add 50% NaOH to adjust the pH to 7, and the temperature is kept at 75℃. 4 hours, cool to 5-10°C, add 5.2 g of sodium acetate (chemically pure, Shijiazhuang Chemical No. 4 Factory) and stir evenly, add 100 g of water after suction filtration, maintain the pH at 7, and heat to 80-85°C. Oxysuccinic acid was precipitated as a white precipitate. Weigh the sodium epoxysuccinate to prepare a 2.0 mol / L aqueous solution, accurately pipette 50 ml of the solution from it, and add it to a four-necked flask with a constant speed stirrer, thermometer and condenser. Heat the ...

Embodiment 2

[0031] Add 49g of maleic anhydride to a four-necked flask equipped with a stirrer and thermometer, add 80ml of deionized water to dissolve it, slowly add 60g of 50% sodium hydroxide solution under stirring at 50℃, control the temperature at 75℃, and then add 1.7g Sodium tungstate and add 65ml of 30% hydrogen peroxide dropwise to the four-necked bottle within about half an hour, add 50% NaOH dropwise to adjust the pH to 7, control the temperature at 80°C and react for 5 hours, then cool to 5°C-15°C, Add 5 grams of cetyltrimethylammonium bromide, stir evenly, add 100 grams of water after suction filtration, maintain the pH value of 7, and heat to 80-85°C. Epoxysuccinic acid appears as a white precipitate. Weigh the Sodium epoxysuccinate is prepared as a 2.0mol / L aqueous solution, 50 ml of solution is accurately pipetted from it, and added to a four-neck flask with a constant speed stirrer, thermometer and condenser, heated to 60°C in an oil bath, and 1.85 g is added Ca(OH) 2 And ...

Embodiment 3

[0034] Add 49g of maleic anhydride to a four-necked flask equipped with a stirrer and thermometer, add 80ml of deionized water to dissolve it, slowly add 60g of 50% sodium hydroxide solution under stirring at 50℃, control the temperature at 75℃, and then add 1.7g Sodium tungstate and add 65ml of 30% hydrogen peroxide dropwise to the four-necked bottle within about half an hour, add 50% NaOH dropwise to adjust the pH to 7, control the temperature at 80°C and react for 5 hours, then cool to 5°C-15°C, Add 4 grams of sodium alanine, stir evenly, add 100 grams of water after suction filtration, maintain the pH at 7, and heat to 80-85°C. Epoxysuccinic acid will precipitate out as a white precipitate. Weigh the sodium epoxysuccinate to prepare It is a 2.0mol / L aqueous solution, from which 50ml of solution is accurately pipetted, and added to a four-necked flask with a constant speed stirrer, thermometer and condenser, heated to 60℃ with an oil bath, and 1.85g of Ca(OH) is added 2 And 0...

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Abstract

The invention discloses a method for synthesizing a polyepoxysuecinic acid salt, which is characterized by comprising the following steps of: dissolving maleic anhydride in deionized water; adding a solution of sodium hydroxide at 30 to 60 DEG C with stirring; adding sodium tungstate and hydrogen peroxide when the temperature is controlled to be between 60 to 100 DEG C; adjusting the pH value to 5 to 7 for reaction for 2 to 100 hours; cooling the reaction solution to below 20 DEG C; adding a precipitator, mixing and stirring the precipitator and the solution; performing suction filtration, adding water into filtrate obtained after suction filtration; keeping the pH value between 6 and 7; heating the filtrate added with water to 70 to 100 DEG C to obtain an epoxysuecinic acid salt; preparing a 0.2 to 4.0 mol / L aqueous solution of the epoxysuecinic acid salt; adding calcium hydroxide and a polymerization promoter into the aqueous solution for performing polymerization reaction till liquid turns yellowish and pasty; and cooling the yellowish and pasty liquid to room temperature to obtain the polyepoxysuccinic acid salt. The method has the advantages of good product quality, low raw material cost and product scale inhibition performance advantageous over that of the prior art.

Description

Technical field [0001] The present invention relates to a method for synthesizing polyepoxysuccinate, and further relates to a method for synthesizing polyepoxysuccinate for water treatment. Background technique [0002] Polyepoxysuccinic acid (PESA) is a new generation of green water treatment agent developed in the 1990s. It is a kind of green scale inhibitor with non-phosphorus, non-nitrogen, good biodegradability and suitable for high alkali and high solid water system. Its scale inhibition effect is obviously better than that of commonly used organic phosphonic acid scale inhibitors. [0003] USP3776850 reported the synthesis of polyepoxysuccinate by the polymerization and re-saponification of diethyl epoxysuccinate catalyzed by boron trifluoride. [0004] USP4654159 discloses the preparation process of polyepoxysuccinic acid. This process is based on maleic anhydride as the raw material. After hydrolysis in an alkaline environment, hydrogen peroxide is added, and sodium hydrox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/22C02F5/10
Inventor 赵冉赵旭赵勇军多文赵新殷冬媛
Owner 北京合创同盛科技有限公司
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