Method for synthesizing polyepoxysuecinic acid salt

A technology of polyepoxysuccinate and epoxysuccinate, which is applied in the field of synthesis of polyepoxysuccinate, can solve the problems of many by-products, low quality of synthetic PESA, and high price of raw materials, so as to overcome the problem of polymerization The degree is not high, which is beneficial to the polymerization reaction and improves the effect of scale inhibition efficiency

Inactive Publication Date: 2009-09-23
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, add tungstic acid Sodium (Nantong Wanbang Science and Technology Fine Chemical Co., Ltd.) 1.7 grams, slowly add 65 milliliters of 30% hydrogen peroxide (Beijing Schindler Chemical Hardware Co., Ltd.), drop 50% NaOH to adjust the pH value to 7, and keep the temperature at 75 ° C for reaction After 4 hours, cool to 5-10°C, add 5.2 grams of sodium acetate (chemically pure, product of Shijiazhuang No. Oxysuccinic acid is precipitated in white, and the sodium epoxysuccinate is weighed to be formulated as a 2.0mol / L aqueous solution, from which 50 milliliters of the solution is accurately pipetted, and added to a four-necked flask with a constant speed stirrer, a thermometer and a condensing device. Heat the oil bath to 60°C and add 1.85 g of Ca(OH)...

Embodiment 2

[0031]Add 49g of maleic anhydride to a four-necked flask equipped with a stirrer and a thermometer, add 80ml of deionized water to dissolve, slowly add 60g of 50% sodium hydroxide solution under stirring at 50°C, control the temperature at 75°C, and then add 1.7g Add sodium tungstate and drop 65ml of 30% hydrogen peroxide into the four-necked bottle within half an hour, add dropwise 50% NaOH to adjust the pH value to 7, control the temperature at 80°C for 5 hours, and cool to between 5°C and 15°C , add 5 grams of cetyltrimethylammonium bromide, stir evenly, add 100 grams of water after suction filtration, maintain the pH value at 7, heat to 80-85 ° C, epoxy succinic acid precipitates out in white, weigh The sodium epoxysuccinate was prepared as a 2.0mol / L aqueous solution, from which 50 ml of the solution was accurately pipetted, added to a four-necked flask equipped with a constant speed stirrer, a thermometer and a condensing device, heated to 60°C with an oil bath, and 1.85 ...

Embodiment 3

[0034] Add 49g of maleic anhydride to a four-necked flask equipped with a stirrer and a thermometer, add 80ml of deionized water to dissolve, slowly add 60g of 50% sodium hydroxide solution under stirring at 50°C, control the temperature at 75°C, and then add 1.7g Add sodium tungstate and drop 65ml of 30% hydrogen peroxide into the four-necked bottle within half an hour, add dropwise 50% NaOH to adjust the pH value to 7, control the temperature at 80°C for 5 hours, and cool to between 5°C and 15°C , add 4 grams of sodium alanine, stir evenly, add 100 grams of water after suction filtration, maintain the pH value at 7, heat to 80-85°C, epoxysuccinic acid precipitates out in white, weigh the sodium epoxysuccinate Prepare a 2.0mol / L aqueous solution, accurately pipette 50ml of the solution, add it to a four-necked flask equipped with a constant speed stirrer, a thermometer, and a condensing device, heat it to 60°C with an oil bath, and add 1.85g of Ca(OH) 2 and 0.05 gram of calci...

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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 kind of synthesis method of polyepoxysuccinate, more particularly relates to the synthesis method of the polyepoxysuccinate used for water treatment. Background technique [0002] Polyepoxysuccinic acid (PESA) is a new generation of green and environmentally friendly water treatment agent developed in the 1990s. It is a green scale inhibitor with the characteristics of no phosphorus, no nitrogen, good biodegradability and suitable for high alkali and high solid water systems. Its antiscalant effect is significantly better than that of commonly used organic phosphonic acid antiscalants. [0003] USP3776850 reported a method for boron trifluoride catalyzed polymerization of diethyl epoxy succinate and saponification to synthesize polyepoxy succinate. [0004] USP4654159 discloses the preparation process of polyepoxysuccinic acid. The process is based on maleic anhydride as raw material. Sodium phosphate is used as a c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/22C02F5/10
Inventor 赵勇军多文赵新
Owner 北京合创同盛科技有限公司
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