CN1294096A

CN1294096A - Process for preparing water-reducing agent

Info

Publication number: CN1294096A
Application number: CN 99117331
Authority: CN
Inventors: 严华; 汪守林; 杨定群; 陈吉明
Original assignee: Chongqing Iron and Steel Group Co Ltd
Current assignee: Chongqing Iron and Steel Group Co Ltd
Priority date: 1999-10-28
Filing date: 1999-10-28
Publication date: 2001-05-09

Abstract

A water-reducing agent is prepared through sulforcating, hydrolyzing, condensating and neutralization. Its advantages low energy consumption as the temp, acidity, feeding speed and pressure are carefully controlled, high quelified rate (100%), and short period.

Description

A kind of production technique of water reducer

The invention belongs to concrete field, particularly a kind of production technique that is used for the water reducer that concrete uses in the cooperation stage.

In building trade, water reducer is a concrete in the indispensable batching that cooperates the stage, makes its consumption that reduces water in engagement process, and moisture content is at solidification stages evaporation formation pore, to reduce concrete density and intensity, satisfy requirements such as pumping in construction, slow setting, strong, expansion early.Adopt water reducer at present on the market, because raw material consumption height in the production process, energy consumption is big, and the process time is long, and qualification rate low (being generally about 60%), so the cost height.

Purpose of the present invention provides a kind of production technique of water reducer.It is raw material consumption ground in process of production, and energy consumption is little, and the production technique time is short, and therefore qualification rate height, the characteristics that cost is low are arranged.

The objective of the invention is to realize with following measure:

Adopt sulfonation, hydrolysis, condensation goes out finished product after the neutralization, it is characterized in that

A. sulfonation: be heated to NAPTHALENE FLAKES. (INDUSTRIAL GRADE and add acid under 150 ℃-175 ℃ and carry out sulfonation, add with 4-16 liter/component velocity, it was fully reacted in constant temperature 120-210 minute, obtain two kinds of naphthene sulfonic acid this moment, and a kind of is α-Nai Huangsuan, and another kind is a beta-naphthalenesulfonic-acid.Wherein the α-Nai Huangsuan instability resolves into naphthalene and acid by hydrolysis with α-Nai Huangsuan.

B. hydrolysis: under 90 ℃-120 ℃, add water, obtained stable beta-naphthalenesulfonic-acid in constant temperature time 18-25 minute with 20-50 liter/component velocity;

C. condensation: (purpose and reaction principle) uses formaldehyde condensation, under 70 ℃-110 ℃, adds formaldehyde with 0.2-0.8 liter/component velocity, and constant temperature time 180-210 minute, so that the chain length that is linked to be of single beta-naphthalenesulfonic-acid is a beta-naphthalenesulfonic-acid more than 6;

D. neutralization: neutralize with caustic soda, the pH value of control solution is about 7-10, under 80 ℃-120 ℃, with the 0.1-1 liter/minute speed add, constant temperature time 10-20 minute, to avoid producing material spray in the N-process.Wherein, make solution be weakly alkaline, react, and in N-process, produce sodium naphthalene sulfonate, i.e. the finished product with the naphthene sulfonic acid reaction to avoid water reducer and cement with the caustic soda neutralization.

E. the above-mentioned raw materials proportioning is (mol ratio) naphthalene: acid: water: formaldehyde=0.8-1.2: 1.0-1.4: 0.2-0.5: 0.6-1.0.

The present invention is because factors such as the temperature in the strict control water reducer production process, acidity, feed rate, pressure can make the energy consumption of product in the whole technology consume coal gas 3000M by 1 ton of product of original every production ³Be reduced to 1 ton of product of present every production and consume coal gas 1500M ³, product percent of pass brings up to 100% by original 60%, the production cycle shortened to 16 hours by original 20 hours, so the production technique time shorten greatly, cost reduces.

The present invention is described further below by embodiment.But the present invention is not limited only to these examples.

Embodiment 1

Press (mol ratio) naphthalene: acid: water: formaldehyde=1.2: 1.4: 0.2: 0.6 proportioning raw materials is got material.At first, after NAPTHALENE FLAKES. (INDUSTRIAL GRADE heated, add sulfuric acid sulfonation at 150 ℃ with 4 liters/minute, acidity control is at PH=2, constant temperature 120 minutes; Adding water for cooling to 90 ℃ controlling acidity with 20 liters/component velocity again is PH=5, and constant temperature 18 minutes makes it produce hydrolysis; Add formaldehyde with 0.2 liter/minute then under 70 ℃, acidity control is carried out condensation PH=5 constant temperature 180 minutes; Add caustic soda with 0.1 liter/minute speed again under 80 ℃ and neutralize, controlling acidity is PH=8, and constant temperature 10 minutes obtains: (1). fishery products (2). and heating, remove moisture content with common drying means and obtain powder product.

Embodiment 2

Press (mol ratio) naphthalene: acid: water: formaldehyde=1.2: 1.4: 0.2: 0.6 proportioning raw materials is got material.At first, after NAPTHALENE FLAKES. (INDUSTRIAL GRADE heated, add sulfuric acid sulfonation at 170 ℃ with 10 liters/minute, acidity is PH=1, constant temperature 180 minutes; Adding water for cooling to 110 ℃ controlling acidity with 35 liters/component velocity again is PH=4, and constant temperature 23 minutes makes it produce hydrolysis; Add formaldehyde with 0.5 liter/component velocity then under 80 ℃, controlling acidity is PH=7, and constant temperature 200 minutes carries out condensation; Add caustic soda with 0.6 liter/minute again under 11 ℃ and neutralize, controlling acidity is PH=10, and constant temperature 17 minutes obtains: (1). fishery products (2). and heating, remove moisture content with common drying means and obtain powder product.

Embodiment 3

Press (mol ratio) naphthalene: acid: water: formaldehyde=0.8: 1: 0.5: 0.6 proportioning raw materials is got material.At first, after NAPTHALENE FLAKES. (INDUSTRIAL GRADE heated, add sulfuric acid sulfonation at 175 ℃ with 16 liters/minute, acidity is PH=2, constant temperature 210 minutes; Adding water for cooling to 120 a ℃ controlling acidity with 90 liters/minute speed again is PH=5, and constant temperature 25 minutes makes it produce hydrolysis; Under 110 ℃, add formaldehyde then with 0.8 liter/minute, controlling acidity PH=5, constant temperature 210 minutes carries out condensation; Add caustic soda with 1 liter/minute speed again under 120 ℃ and neutralize, controlling acidity is PH=7, and constant temperature 20 minutes obtains: (1). fishery products (2). and heating is removed moisture content with common drying means and is obtained powder product.

Claims

1. the production technique of a water reducer adopts sulfonation, hydrolysis, and condensation goes out finished product after the neutralization, it is characterized in that

A. sulfonation: be heated to NAPTHALENE FLAKES. (INDUSTRIAL GRADE and add sulfuric acid under 150 ℃-175 ℃ and carry out sulfonation, add, it was fully reacted in constant temperature 120-210 minute with 4-16 liter/component velocity;

B. hydrolysis: water adds constant temperature time 18-25 minute with 20-50 liter/component velocity under 90 ℃-120 ℃;

C. condensation: use formaldehyde condensation, under 70 ℃-110 ℃, add formaldehyde, constant temperature time 180-210 minute with 0.2-0.8 liter/component velocity;

D. neutralization: neutralize with caustic soda, the pH value of control solution is about 7-10, under 80 ℃-120 ℃, with the 0.1-1 liter/minute speed add constant temperature time 10-20 minute;