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 reducer, which is applied in the direction of sulfonic acid preparation, chemical instruments and methods, physical/chemical process catalysts, 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 reducing performance, and improve the effect of water reducing rate

Active Publication Date: 2022-07-15
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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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

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Experimental program
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Effect test

Embodiment 1

[0036] Step 1) At 25°C, add 50g of polyethylbenzene column bottom high boiler and 50g of 98wt% concentrated sulfuric acid into the reaction kettle, after reacting at 135°C for 4h, stand for stratification, collect the lower layer liquid, polyethylbenzenesulfonic acid ;

[0037] Step 2) At 25°C, add 2.0g fumed silica and 100g deionized water to the reaction kettle, react at 80°C for 2h, add 12g 1wt.% N-[3-(trimethoxysilyl)propane] After continuing to react for 6h, filter the filter cake, wash the filter cake with 180g ethanol, and then dry it at 80°C for 24h to obtain modified silica;

[0038] Step 3) At 25°C, 0.3 g of sodium metaaluminate, 3.0 g of anhydrous sodium hydroxide, 1.6 g of the modified silica prepared in step 2), 3.6 g of N,N,N-trimethyl- 1-adamantanamine, 1.5g carbon nanotubes, 0.6g (2,2'-bipyridine) nickel diiodide were added to the reaction kettle, 400W microwave was reacted at 120°C for 5d, filtered, and the filter cake was washed with deionized water until T...

Embodiment 2

[0045] Step 1) At 25°C, add 60g of polyethylbenzene column bottom high boiler and 55g of 98wt% concentrated sulfuric acid into the reaction kettle, after reacting at 120°C for 2.5h, stand for stratification, collect the lower layer liquid, polyethylbenzenesulfonic acid acid;

[0046] Step 2) At 25°C, add 2.5g fumed silica and 125g deionized water into the reaction kettle, react at 85°C for 1.5h, add 12.5g 3wt.% N-[3-(trimethoxysilyl) ) propyl]aniline in methanol, continue to react for 6.5h, filter, wash the filter cake with 250g 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 the modified silica prepared in step 2), 4g of N,N,N-trimethyl-1- Amantadine, 1.8g carbon nanotubes, 0.7g (2,2'-bipyridine) nickel diiodide were added to the reaction kettle, 500W microwave was reacted at 130°C for 5d, filtered, and the filter cake was washed with deionized water until the pH of ...

Embodiment 3

[0051] Step 1) At 25°C, add 30g of polyethylbenzene tower bottom high boiler and 30g of oleum into the reaction kettle, after reacting at 90°C for 8h, stand for stratification, collect the lower layer liquid, polyethylbenzenesulfonic acid;

[0052] Step 2) At 25°C, add 4g of fumed silica and 200g of deionized water into the reaction kettle, react at 75°C for 2h, add 20g of 1wt.% vinyltriethoxysilane methanol solution, and continue to react 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, mix 0.1 g of sodium metaaluminate, 1 g of anhydrous sodium hydroxide, 0.5 g of the modified silica prepared in step 2), 1.2 g of N,N,N-trimethyl-1 -Amantadine, 0.5g carbon nanotubes, 0.2g (2,2'-bipyridine) nickel diiodide were added to the reaction kettle, 500W microwave was reacted at 100°C for 3d, filtered, and the filter cake was washed with deionized water to filtrate The pH was 7, and dried at 80 °...

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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, and the polyethylbenzene sulfonic acid is prepared by sulfonating 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 molecules are practically applied to the building field and have 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 building admixtures, and in particular relates to a method for preparing a polyether polycarboxylic acid type high-efficiency water reducer from a high-boiling substance at the bottom of a polyethylbenzene tower. Background technique [0002] Ethylbenzene is an important petrochemical basic raw material. It is mainly synthesized by catalytic alkylation of high-purity ethylene and benzene. It 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, resulting in polyethylbenzene (diethylbenzene to hexaethylbenzene), diphenylethane, diphenylmethane and other high boiling points. The by-products remain at the bottom of the rectifying tower, and the average molecular mass of the high boilers at the bottom of the polyethylbenzene tower remaining at the bottom of the ethylbenzene tower is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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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