CN101314556A - Process for recovering residual naphthalin in naphthalin series water reducing agent synthesis - Google Patents

Abstract

The invention relates to a method for recovering residual naphthalene during the synthesizing process of naphthalene water reducing agent and the naphthalene water reducing agent used for cement concrete. The invention provides a simple method for recovering the naphthalene, namely the method for recovering the residual naphthalene by arrangement of apparatuses on the basis of sulfonation reaction in the prior synthetic technological flow, aiming at the fact that the prior produced naphthalene water reducing agent adopts the synthetic technological flow of sulfonation, hydrolysis, condensation, neutralization and so on and the prior manufacturing technique has severe defects and can not completely react naphthalene during the process of the sulfonation reaction. The method adopts the technical proposal that: water vapor with 0.1 to 0.3 MPa enters into a sulfonation reaction kettle so as to make materials in the kettle boil, and the residual naphthalene in the kettle which is not completely reacted flows out in the gaseous state; and the recovered naphthalene is obtained after temperature reduction, dissolution, filtration and centrifugal dewatering.

Description

The recovery method of residual naphthalene during naphthalene water reducer is synthetic

One, technical field

The present invention relates to the recovery method of the synthetic middle residual naphthalene of naphthalene water reducer, especially naphthalene water reducer of cement concrete use.

Two, background technology

Naphthalene water reducer is that utilization is widest in area in the high efficiency water reducing agent at present, the usage quantity maximum, it also is the concrete admixture of turnout maximum, according to incompletely statistics, nearly more than the 30 ten thousand tons of naphthalene water reducer pulvis of whole nation annual production, its production technique comparative maturity adopts synthesis techniques such as sulfonation, hydrolysis, condensation, neutralization to form.

But this technology has major defect; can't in the sulfonation reaction process, naphthalene be reacted completely; there is the naphthalene about 8% to residue in the water reducer; not only the effect of naphthalene can not get fully playing and utilizing; and also have the smell of naphthalene in the water reducer, and human body there is in various degree harm, be unfavorable for the protection of environment; the value of naphthalene is expensive at present simultaneously, reaches about 9 yuan/kilogram.By dropping into about about 39% the naphthalene of 6500 kilograms of concentration of 1000 kilograms of naphthalene production is that aqua reclaims minimum 6% estimation of naphthalene, reclaim 60 kilograms of naphthalenes, be worth 540 yuan, aqua per ton is saved 83 yuan of costs, about 210 yuan of pulvis saving per ton, for producing the big enterprise of naphthalene water reducer amount, annual escapable cost is more than more than 1,000 ten thousand yuan, and technical economic benefit is very remarkable.

Three, summary of the invention

The purpose of this invention is to provide the simple method that a kind of naphthalene reclaims, is to increase equipment configuration to reclaim residual naphthalene 5-8% in original synthesis technique flow process sulfonation reaction, to reduce cost; increase the benefit; strengthen Enterprises'Competitiveness, economize on resources, the human environment of depending on for existence of protection.

The technical solution adopted in the present invention, its recovery method and step are as follows:

Import steam under pressure in a, the sulfonation reaction still: the bottom at the sulfonation reaction still is communicated with steam-pipe, 0.1-0.3MPa in the straight-through sulfonation reaction still of the steam of pressure, make the feed liquid boiling in the sulfonation reaction still, the logical 1-3 hour steam time, make the residual naphthalene that does not thoroughly react in the sulfonation reaction still enter the pipeline on sulfonation reaction still top with gaseous form, keep sulfonation reaction still interlayer to be connected with steam simultaneously, the temperature in the sulfonation reaction still is 160 ℃--165 ℃;

B, naphthalene reclaim: the gasiform naphthalene flows in the naphthalene recovery still from the pipeline on sulfonation reaction still top, naphthalene reclaims the interior water management of still 1/2nd, the sulfonation reaction still is produced 8-12 water reducer, naphthalene can be reclaimed the pipeline valve of still bottom opens, make the aqueous solution that is dissolved with naphthalene flow into filtering basin, the non-naphthalene gas that naphthalene reclaims in the still flows to condenser through naphthalene recovery still upper pipe;

C, filter dehydration: the solution that contains naphthalene that flows out from naphthalene recovery still flows into the filtering basin, and 80 orders-100 purpose filtering net is arranged on the filtering basin, and filtered solution enters whizzer and dewaters, and promptly get and reclaim naphthalene, the water that whizzer is deviate from, reusable;

D, condensation: naphthalene reclaims the non-naphthalene gas in the still, reclaims still upper pipe inflow condenser through naphthalene and carries out heat exchange, makes the gas cooling of inflow, through the gas of cooling, flows into the deodorizing jar by pipeline;

E, deodorizing: enter the gas water spray cleaning in the deodorizing jar, further reduce the temperature of gas, in the jar of deodorizing simultaneously a small amount of liquid caustic soda is housed, carry out neutralizing treatment, it is neutral, reusable that the water after the neutralization is, emptying pipe is equipped with in deodorizing jar upper end, carries out emptying.

The present invention, it is simple to have a recovery process, characteristics such as equipment is easy to get, and cost is low, and recovering effect is obvious.

Four, description of drawings

Further specify the present invention in conjunction with the accompanying drawings.

Accompanying drawing is a process flow diagram of the present invention.

Among the figure: 1-sulfonation reaction still 2-naphthalene reclaims still 3-condenser 4-deodorizing jar 5-filtering basin 6-whizzer 7-naphthalene 8-steam pipeline 9-pipeline 10-evacuated tube

Five, embodiment

Further specify the present invention below in conjunction with examples of implementation.0.15MPa the straight-through sulfonation reaction still of steam in, 2 hours time, make the liquid boiling in the sulfonation reaction still, thoroughly the residual naphthalene of reaction does not reclaim in the still with the pipeline inflow naphthalene that gaseous form is communicated with from sulfonation reaction still top, the sulfonation reaction temperature in the kettle is 160 ℃, in naphthalene reclaims still, 1/2nd water is arranged, when the sulfonation reaction still is produced 10 water reducers, open naphthalene and reclaim still bottom valve, make naphthalene solution flow into filtering basin, there are 100 purpose filtering nets to filter on the filtering basin, enter whizzer after the filtration again and dewater, promptly get and reclaim naphthalene; The non-naphthalene gas that naphthalene reclaims in the still carries out heat exchange from the pipeline inflow condenser that naphthalene reclaims the connection of still top, the cooling back flows into the deodorizing jar by pipeline and sprays, purifies, lowers the temperature, simultaneously, in the deodorizing jar liquid caustic soda is arranged, carry out neutralizing treatment, remaining gas is discharged from the evacuated tube of deodorizing jar upper end; Zhong Heshui in water that whizzer is deviate from and the deodorizing jar, reusable.

Claims (1)

1, the recovery method of the synthetic middle residual naphthalene of a kind of naphthalene water reducer is characterized in that recovery method and step are as follows:

Import steam under pressure in a, the sulfonation reaction still: the bottom at the sulfonation reaction still is communicated with steam-pipe, 0.1-0.3MPa in the straight-through sulfonation reaction still of the steam of pressure, make the feed liquid boiling in the sulfonation reaction still, the logical 1-3 hour steam time, make the residual naphthalene that does not thoroughly react in the sulfonation reaction still enter the pipeline on sulfonation reaction still top with gaseous form, keep sulfonation reaction still interlayer to be connected with steam simultaneously, the temperature in the sulfonation reaction still is 160 ℃--165 ℃;

B, naphthalene reclaim: the gasiform naphthalene flows in the naphthalene recovery still from the pipeline on sulfonation reaction still top, naphthalene reclaims the interior water management of still 1/2nd, the sulfonation reaction still is produced 8-12 water reducer, naphthalene can be reclaimed the pipeline valve of still bottom opens, make the aqueous solution that is dissolved with naphthalene flow into filtering basin, the non-naphthalene gas that naphthalene reclaims in the still flows to condenser through naphthalene recovery still upper pipe;

C, filter dehydration: the solution that contains naphthalene that flows out from naphthalene recovery still flows into the filtering basin, and 80 orders-100 purpose filtering net is arranged on the filtering basin, and filtered solution enters whizzer and dewaters, and promptly get and reclaim naphthalene, the water that whizzer is deviate from, reusable;

D, condensation: naphthalene reclaims the non-naphthalene gas in the still, reclaims still upper pipe inflow condenser through naphthalene and carries out heat exchange, makes the gas cooling of inflow, through the gas of cooling, flows into the deodorizing jar by pipeline;

E, deodorizing: enter the gas water spray cleaning in the deodorizing jar, further reduce the temperature of gas, in the jar of deodorizing simultaneously a small amount of liquid caustic soda is housed, carry out neutralizing treatment, it is neutral, reusable that the water after the neutralization is, emptying pipe is equipped with in deodorizing jar upper end, carries out emptying.