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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  • 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

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

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0035] Example 1

[0036] At step 1) 25 ℃, 50g of high boiling bottoms polyethylbenzenes and 50g 98wt% of concentrated sulfuric acid added to the kettle, the reaction at 135 deg.] C for 4h, allowed to stand stratification, the lower liquid collection, much ethylbenzene sulfonic acid ;

[0037] Under Step 2) 25 ℃, the fumed silica and 2.0g 100g of deionized water was added to the kettle, 80 ℃ reaction for 2h, 12g 1wt.% Of N- [3- (trimethoxysilyl silicon) propan after methanol-yl] aniline, the reaction was continued for 6h, filtered and the filter cake was washed with 180g of ethanol and dried 80 deg.] C 24h, to obtain the modified silica;

[0038] The step 3) 25 ℃, 0.3g sodium aluminate, 3.0g of anhydrous sodium hydroxide, 1.6g Step 2) prepared in modified silica, 3.6g N, N, N- trimethyl - 1-adamantanamine, 1.5 g carbon nanotubes, 0.6g (2,2'- bipyridine) nickel diiodide was added to the reaction kettle, 120 ℃ 400W microwave reaction 5D, filtered, and the filter cake was washed with...

Example Embodiment

[0044] Example 2

[0045] At step 1) 25 ℃, 60g of high boiling bottoms polyethylbenzenes and 55g 98wt% of concentrated sulfuric acid added to the kettle, the reaction at 120 deg.] C for 2.5h, allowed to stand stratification, the lower liquid collection, much ethylbenzene sulfonamide acid;

[0046] Under Step 2) 25 ℃, 2.5g of fumed silica and 125g of deionized water was added to the reaction kettle, the reaction 1.5h 85 ℃, was added 12.5g 3wt.% Of N- [3- (trimethoxysilyl silicon after) methanol propyl] aniline, the reaction was continued for 6.5h, filtered and the filter cake was washed with 250g of ethanol and dried 85 ℃ 24h, to obtain the modified silica;

[0047] The step 3) 25 ℃, 0.5g sodium aluminate, 5g of anhydrous sodium hydroxide, 2.6g Step 2) prepared in modified silica, 4g N, N, N- trimethyl-1 amantadine, 1.8 g of carbon nanotube, 0.7g (2,2'- bipyridine) nickel diiodide was added to the reaction kettle, 130 ℃ 500W microwave reaction 5D, filtered, and the filter cake was ...

Example Embodiment

[0050] Example 3

[0051] At step 1) 25 ℃, 30g of high boiling bottoms polyethylbenzenes and 30g fuming sulfuric acid added to the kettle, the reaction after 8h at 90 ℃, standing layer, the lower liquid collection, much acetic acid;

[0052] Under Step 2) 25 ℃, 4g of fumed silica and 200g of deionized water was added to the reaction kettle, the reaction 2h 75 ℃, methanol was added a solution of 20g 1wt.% Of vinyltriethoxysilane, and the reaction was continued for 6h , filtered, and the filter cake was washed with 500g of ethanol and dried 90 deg.] C 24h, to obtain the modified silica;

[0053] The step 3) 25 ℃, 0.1g sodium aluminate, 1g of anhydrous sodium hydroxide, 0.5g Step 2) prepared in modified silica, 1.2g N, N, N- trimethyl-1 - amantadine, carbon nanotubes 0.5g, 0.2g (2,2'- bipyridine) nickel diiodide was added to the reaction kettle, 100 ℃ 500W microwave reaction 3d, filtered, and the filter cake was washed with deionized water until the filtrate pH of 7,80 ℃ dried 12h, S...

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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
CPCC08F283/065C08F2/46C08F2/38C08F4/80C08F4/02C07C303/22B01J31/0244B01J31/0271C04B24/165C07C2601/14B01J2231/4205C04B2103/302C07C309/44C08F216/36C08F220/06
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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