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Method for preparing polyether polycarboxylic acid type high-efficiency water reducing agent from polyethylbenzene tower bottom high-boiling residues

A technology of polyether polycarboxylic acid and high-efficiency water reducing agent, which is applied in the preparation of sulfonic acid, chemical instruments and methods, catalysts for physical/chemical processes, etc., can solve the problems of high industrialization cost, large amount of benzene, and high impurity content in products. Achieve good industrial application prospects, improve water reduction performance, and improve the effect of water reduction rate

Active Publication Date: 2021-11-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese patents CN11701096A and CN1310051A disclose a method for gas-phase alkylation transfer of polyethylbenzene and its catalyst, but the activity of the catalyst is low, the amount of benzene used in the alkylation reaction is large, and the impurity content of the product is high. In addition, the The process of converting polyethylbenzene into ethylbenzene consumes a lot of energy, and the cost of industrialization is high, so it is difficult to apply

Method used

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  • Method for preparing polyether polycarboxylic acid type high-efficiency water reducing agent from polyethylbenzene tower bottom high-boiling residues
  • Method for preparing polyether polycarboxylic acid type high-efficiency water reducing agent from polyethylbenzene tower bottom high-boiling residues
  • Method for preparing polyether polycarboxylic acid type high-efficiency water reducing agent from polyethylbenzene tower bottom high-boiling residues

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Step 1) At 25°C, add 50g polyethylbenzene tower bottom high boilers and 50g 98wt% concentrated sulfuric acid into the reaction kettle, react at 135°C for 4h, let stand to separate layers, collect the lower liquid, polyethylbenzenesulfonic acid ;

[0037] Step 2) At 25°C, add 2.0g of fumed silica and 100g of deionized water into the reactor, react at 80°C for 2h, add 12g of 1wt.% N-[3-(trimethoxysilyl)propane Base] methanol solution of aniline, continue to react for 6 hours, filter, wash the filter cake with 180g ethanol and dry at 80°C for 24 hours to obtain modified silica;

[0038] Step 3) At 25°C, 0.3g of sodium metaaluminate, 3.0g of anhydrous sodium hydroxide, 1.6g of the modified silica prepared in step 2), 3.6g of N,N,N-trimethyl- Add 1-adamantanamine, 1.5g carbon nanotubes, and 0.6g (2,2'-bipyridine) nickel diiodide into the reaction kettle, react with 400W microwave at 120°C for 5d, filter, and wash the filter cake with deionized water until The pH of the fil...

Embodiment 2

[0045] Step 1) At 25°C, add 60g of polyethylbenzene tower bottom high boilers and 55g of 98wt% concentrated sulfuric acid into the reaction kettle, react at 120°C for 2.5h, let stand to separate layers, collect the lower liquid, polyethylbenzenesulfonate acid;

[0046] Step 2) At 25°C, add 2.5g of fumed silica and 125g of deionized water into the reactor, react at 85°C for 1.5h, add 12.5g of 3wt.% N-[3-(trimethoxysilyl ) methanol solution of propyl]aniline, continue to react for 6.5h, filter, wash the filter cake with 250g of ethanol and dry at 85°C for 24h to obtain modified silica;

[0047] Step 3) At 25°C, 0.5g of sodium metaaluminate, 5g of anhydrous sodium hydroxide, 2.6g of modified silica prepared in step 2), 4g of N,N,N-trimethyl-1- Add amantadine, 1.8g carbon nanotubes, and 0.7g (2,2'-bipyridine) nickel diiodide into the reaction kettle, react with 500W microwave at 130°C for 5d, filter, and wash the filter cake with deionized water to the pH of the filtrate 7, drie...

Embodiment 3

[0051] Step 1) At 25°C, add 30g of polyethylbenzene tower bottom high boiler and 30g of fuming sulfuric acid into the reaction kettle, react at 90°C for 8h, let stand to separate layers, collect the lower liquid, polyethylbenzenesulfonic acid;

[0052] Step 2) At 25°C, add 4g of fumed silica and 200g of deionized water into the reactor, react at 75°C for 2h, add 20g of 1wt.% methanol solution of vinyltriethoxysilane, and continue the reaction for 6h , filtered, washed the filter cake with 500g ethanol and dried at 90°C for 24h to obtain modified silica;

[0053] Step 3) At 25°C, 0.1g of sodium metaaluminate, 1g of anhydrous sodium hydroxide, 0.5g of the modified silica prepared in step 2), 1.2g of N,N,N-trimethyl-1 - Add amantadine, 0.5g carbon nanotubes, 0.2g (2,2'-bipyridine) nickel diiodide into the reaction kettle, react with 500W microwave at 100°C for 3d, filter, wash the filter cake with deionized water to the filtrate pH is 7, dried at 80°C for 12 hours to obtain SSZ-...

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Abstract

The invention relates to a method for preparing a polyether polycarboxylic acid type high-efficiency water reducing agent from polyethylbenzene tower bottom high-boiling residues. The polyether polycarboxylic acid type high-efficiency water reducing agent is prepared by free radical polymerization of arone olefin, a double-bond-containing macromonomer and a micromolecular monomer, and the arone olefin is prepared by catalytic acylation of poly-ethylbenzene sulfonic acid and unsaturated acylate by using a bifunctional molecular sieve encapsulated catalyst. The bifunctional molecular sieve encapsulated catalyst is prepared by one-step hydrothermal reaction of sodium metaaluminate, sodium hydroxide, modified silicon dioxide, N,N,N-trimethyl-1-amantadine, carbon nanotubes and (2,2'-bipyridine) nickel diiodide. The polyethylbenzene sulfonic acid is prepared by sulfonating the high-boiling residues at the bottom of a polyethylbenzene tower. According to the method, the polyethylbenzene tower bottom high-boiling residues serve as raw materials, polyether polycarboxylic acid type high-efficiency water reducing agent molecules are prepared through the steps of sulfonation, acylation, free radical polymerization and the like, and the polyether polycarboxylic acid type high-efficiency water reducing agent is practically applied to the building field and has important significance in resourceful treatment of the ethylbenzene tower bottom high-boiling residues.

Description

technical field [0001] The invention belongs to the technical field of construction admixtures, and in particular relates to a method for preparing polyether polycarboxylate high-efficiency water reducers from polyethylbenzene tower bottom high boilers. Background technique [0002] Ethylbenzene is an important petrochemical basic raw material, which is mainly synthesized by the catalytic alkylation reaction of high-purity ethylene and benzene, and is the main raw material for the production of styrene. In addition to the selective alkylation of benzene and ethylene to generate ethylbenzene, many side reactions will also occur to generate polyethylbenzene (diethylbenzene to hexaethylbenzene), diphenylethane, diphenylmethane and other high boiling point The by-products remain in the bottom of the rectification tower, and the average molecular weight of the high boilers at the bottom of the ethylbenzene tower is 180-210. Because the composition of the high boilers at the botto...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F216/36C08F220/06C08F2/46C08F2/38C08F4/80C08F4/02C07C303/22C07C309/44B01J31/02C04B24/16C04B103/30
CPCC08F283/065C08F2/46C08F2/38C08F4/80C08F4/02C07C303/22B01J31/0244B01J31/0271C04B24/165C07C2601/14B01J2231/4205C04B2103/302C07C309/44C08F216/36C08F220/06Y02W30/91
Inventor 周钰明唐晓伟鲍杰华石旵东葛素娟肖海平邱磊杨森王润东黄镜怡
Owner CHINA PETROLEUM & CHEM CORP
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