A kind of preparation method of sulfamic acid series water reducer

Abstract

The invention relates to the technical field of production of cement additives and in particular relates to a preparation method of an aminosulfonic acid based water reducing agent. The preparation method comprises a pre-treatment step of phenol-containing wastewater; a combined type extracting solvent is adopted so that the extracting efficiency is improved; the water reducing agent is prepared from raw materials including crude phenol, sodium, caustic soda flakes and an FePO4 solid acid catalyst; the reaction time is greatly shortened and the conversion rate of the raw materials is improved;and the preparation method further comprises post-treatment of the water reducing agent, so that the purity of a reaction product is further improved. According to the aminosulfonic acid based waterreducing agent prepared by utilizing the preparation method, wastes can be utilized, and the convenient and economical aminosulfonic acid based efficient water reducing agent also can be improved; andthe aminosulfonic acid based water reducing agent has a wide application prospect and market value.

Description

technical field

[0001] The invention relates to the technical field of cement admixture production, in particular to a preparation method of a sulfamic acid-based water reducer. Background technique

[0002] The discharge of a large amount of phenolic wastewater has caused obvious harm to the aquatic ecosystem. Phenol-containing wastewater mainly comes from coking plants, gas plants, petrochemical plants, insulation material plants and other industrial sectors, as well as the production process of petroleum cracking to ethylene, synthetic phenol, polyamide fiber, synthetic dyes, organic pesticides and phenolic resin. The way to solve phenol-containing wastewater in industrial production is to actively promote clean production to reduce the amount of waste; secondly, to strengthen terminal treatment. Once phenol-containing wastewater is discharged from the production device, it must be recycled as much as possible, and it must be treated to meet the standard. emission. The ...

Examples

Embodiment 1

[0022] (1) Pretreatment of phenol-containing wastewater; (i) removing impurities in phenol-containing wastewater by coarse filtration; (ii) 500 g of methyl isobutyl ketone, 130 g of sodium alginate, and N,N dimethylformamide The mixed solution of 150mL and 78g of butyl carbonate is used as the extractant and the phenol-containing wastewater treated in step (i) is loaded into the extraction container according to the volume ratio of 1:5, stirred rapidly at 50°C for 15min and then allowed to stand for 60min; (iii) The solution after step (ii) standing still is separated into the lower raffinate phase and the upper extract phase, and gas chromatography is used to analyze the content of phenolic substances in the raffinate phase to obtain crude phenol.

[0023] (2) Preparation of water reducer: (i) Add 450g of crude phenol obtained in step (1) and 50g of para-sodium to water in sequence, then add 1g of caustic soda until the pH value of the mixture is adjusted to 8, and add 90g of ...

Embodiment 2

[0027] (1) Pretreatment of phenol-containing wastewater; (i) removing impurities in phenol-containing wastewater by coarse filtration; (ii) 200 g of methyl isobutyl ketone, 50 g of sodium alginate, and N,N dimethylformamide The mixed solution of 75mL and 30g of butyl carbonate is used as the extractant and the phenol-containing wastewater treated in step (i) is loaded into the extraction container according to the volume ratio of 1:4, and it is stirred rapidly at 50°C for 15 minutes and then allowed to stand for 60 minutes; (iii) The solution after step (ii) standing still is separated into the lower raffinate phase and the upper extract phase, and gas chromatography is used to analyze the content of phenolic substances in the raffinate phase to obtain crude phenol.

[0028] (2) Preparation of water reducer: (i) Add 400 g of crude phenol obtained in step (1) and 45 g of para-sodium to water in sequence, then add 0.8 g of caustic soda until the pH value of the mixture is adjuste...

technical field

[0001] The invention relates to the technical field of cement admixture production, in particular to a preparation method of a sulfamic acid-based water reducer. Background technique

[0002] The discharge of a large amount of phenolic wastewater has caused obvious harm to the aquatic ecosystem. Phenol-containing wastewater mainly comes from coking plants, gas plants, petrochemical plants, insulation material plants and other industrial sectors, as well as the production process of petroleum cracking to ethylene, synthetic phenol, polyamide fiber, synthetic dyes, organic pesticides and phenolic resin. The way to solve phenol-containing wastewater in industrial production is to actively promote clean production to reduce the amount of waste; secondly, to strengthen terminal treatment. Once phenol-containing wastewater is discharged from the production device, it must be recycled as much as possible, and it must be treated to meet the standard. emission. The ...

Examples

Embodiment 1

[0022] (1) Pretreatment of phenol-containing wastewater; (i) removing impurities in phenol-containing wastewater by coarse filtration; (ii) 500 g of methyl isobutyl ketone, 130 g of sodium alginate, and N,N dimethylformamide The mixed solution of 150mL and 78g of butyl carbonate is used as the extractant and the phenol-containing wastewater treated in step (i) is loaded into the extraction container according to the volume ratio of 1:5, stirred rapidly at 50°C for 15min and then allowed to stand for 60min; (iii) The solution after step (ii) standing still is separated into the lower raffinate phase and the upper extract phase, and gas chromatography is used to analyze the content of phenolic substances in the raffinate phase to obtain crude phenol.

[0023] (2) Preparation of water reducer: (i) Add 450g of crude phenol obtained in step (1) and 50g of para-sodium to water in sequence, then add 1g of caustic soda until the pH value of the mixture is adjusted to 8, and add 90g of ...

Embodiment 2

[0027] (1) Pretreatment of phenol-containing wastewater; (i) removing impurities in phenol-containing wastewater by coarse filtration; (ii) 200 g of methyl isobutyl ketone, 50 g of sodium alginate, and N,N dimethylformamide The mixed solution of 75mL and 30g of butyl carbonate is used as the extractant and the phenol-containing wastewater treated in step (i) is loaded into the extraction container according to the volume ratio of 1:4, and it is stirred rapidly at 50°C for 15 minutes and then allowed to stand for 60 minutes; (iii) The solution after step (ii) standing still is separated into the lower raffinate phase and the upper extract phase, and gas chromatography is used to analyze the content of phenolic substances in the raffinate phase to obtain crude phenol.

[0028] (2) Preparation of water reducer: (i) Add 400 g of crude phenol obtained in step (1) and 45 g of para-sodium to water in sequence, then add 0.8 g of caustic soda until the pH value of the mixture is adjuste...