CN207659355U - Phenyl guanidine carbonate recovery device in waste water - Google Patents

Abstract

The utility model provides phenyl guanidine carbonate recovery device in a kind of waste water, has by the sequentially connected centrifuge of flow, water tank, membrane filter, addition reaction kettle, phenyl guanidine carbonate follow-up equipment；There is solid inlet, hydrochloric acid entrance, reacting product outlet on addition kettle.Water circulating pump is connected between centrifuge and water tank.The device application method is then to obtain final products phenyl guanidine carbonate by first generating guanidines hydrochloride.Effective solid in waste water can be become phenyl guanidine carbonate by the utility model by being acidified and replacing reaction, and useful component is fully recycled.

Description

Phenyl guanidine carbonate recovery device in waste water

Technical field

The utility model belongs to the treatment technology of the water containing solid waste.

Background technology

Phenyl guanidine carbonate is white, needle-shaped crystals or pulverulent solids.149-153 DEG C of fusing point, is slightly soluble in water, is dissolved in heat Water, ethyl alcohol, acetone and other organic solvent.Molecular formula:（C7H9N3）2H2CO3.Phenyl guanidine carbonate is synthesis miazines medicine production The important intermediate of the fine chemicals such as product, heterocyclic dyestuff and agricultural chemical insecticide.

Phenyl guanidine hydrochloride, the synthetic reaction formula of phenyl guanidine carbonate are as follows：

Guanidines wastewater treatment generally uses two ways at present：

A kind of basic principle detaching aniline and guanidines in guanidines waste water by liquid membrane emulsion technology, is aniline And guanidines can be dissolved in film phase, it passes through film phase diffusive migration under the effect of interior outer aqueous phase concentration difference from film phase high concentration side It to low concentration side, reacts with the acid in inner aqueous phase, produces aniline hydrochlorate, then recycle.But the solid in waste water is not It can be recycled, and this kind of method cost of disposal is higher；

Another way is exactly the unified recycling solid by settling waste water, then is turned guanidines by chain control pH It is melted into phenyl guanidine hydrochloride liquid, bisguanides, urea these solids are fallen in press filtration, then useless will admittedly burn, phenyl guanidine hydrochloride It is recycled in production phenyl guanidine carbonate.

Number of patent application provides a kind of new synthetic method of phenylguanidine bicarbonate for 2013100816049 invention, This method uses aniline for starting material, and aniline bicarbonate is synthesized with carbon dioxide reaction, then with cyanamide solution in dioxy Change and reacts synthesis of phenyl guanidine bicarbonate under carbon system.The invention does not provide processing method to the waste water after synthetic reaction, has Larger environmental problem.

The invention that number of patent application is 2012103016197 is related to the technology of preparing of pyrimethanil.With aniline, cyanamide and second Acyl acetone is raw material, includes at least guanidine salt preparation, acidity adjustment and cyclisation and last handling process, it is characterised in that：With C2~C5 Monohydric alcohol be solvent, under the conditions of pH3~4, chlorination hydrogen catalysis prepares phenyl guanidine hydrochloride, without isolation depositing in organic base It is directly reacted with acetylacetone,2,4-pentanedione lower, obtains pyrimethanil.The recyclable alcohol of the filtered mother liquor of this method is reused, but to solid Useless that materials is waited not to be recycled, processing is not thorough enough.

Invention content

Purpose of utility model：

Phenyl guanidine carbonate recovery device in a kind of waste water is provided, the solid content in waste water is reduced, mitigates chemical industry enterprise The pressure of three-protection design in industry, while improving product yield.

Technical solution：Phenyl guanidine carbonate recovery device in the waste water that this case provides has and is sequentially connected by flow Centrifuge, water tank, membrane filter, addition reaction kettle, phenyl guanidine carbonate follow-up equipment.It is connected between centrifuge and water tank There is water circulating pump；There is solid inlet, hydrochloric acid entrance on addition kettle（The inlet has control valve）, reacting product outlet, It is another to there is PH to count socket, PH meters and control valve chain control, pass through the inlet of the metering regulation and control hydrochloric acid of pH value.

The device uses the recovery process step of following sequence：

（1）By phenyl guanidine carbonate（Predominantly phenyl guanidine carbonate, bisguanides, urea and sodium carbonate）Centrifuge mother liquor it is complete Portion is collected into the water tank with segmentation partition board, and the solid in mother liquor is allowed to carry out free settling（Sedimentation time is 12 hours left sides It is right）, the liquid material not settled flows through the membrane filtration containing micropore so that the solid content to suspend in liquid material is by 2.3 ‰ Left and right drops to 0.1 ‰ or so, ensures that solid material fully filters out, collects solid in filter membrane micropore；So that miscible in liquid A small amount of solid is recycled, and ensures that final yield is higher, reduces waste and discharge.

（2）Material will be periodically deposited in water tank, and nitrogen bubbling is discharged by the nitrogen device of bottom（Water tank bottom has nitrogen Bubbling device.When needing periodic cleaning, be bubbled -10 minutes 5 minutes, be then delivered to centrifuge, such time interval ensure compared with High production efficiency of working continuously, and ensure solid cleaning ratio more thoroughly）, it is transported in centrifuge, is separated by solid-liquid separation again；

（3）It will（1）With（2）The solid being collected into is thrown into addition kettle, is acidified by hydrochloric acid, and pH is controlled in 4.5-5.0, salt The aperture of sour inlet valve and the chain regulation and control of pH on-line checkings, prevent salt excessive acid（Excessive acid will cause solution to be in larger acidity, no Conducive to the formation of follow-up carbonate, the rate of recovery reduces.Subacidity, it is impossible to be that aniline is completely converted into phenyl guanidine hydrochloride, most The phenyl guanidine carbonate yield formed afterwards is also relatively low）, the by-products such as bisguanides, urea are then fallen by filtering equipment press filtration, are recycled Phenyl guanidine hydrochloride.Then subsequent process production is carried out by phenyl guanidine hydrochloride again, obtains final products phenyl guanidine carbonate.

（4）Waste water after phenyl guanidine hydrochloride to guanidines carbonate reaction is the waste water that centrifuge generates, and is returned to Step（1）In, continue to apply mechanically in cycles.

Advantageous effect：

The utility model proposes this modes of water process containing solid waste, can be by effective solid in waste water by being acidified and replacing Reaction becomes phenyl guanidine carbonate, and useful component is fully recycled, and the yield of guanidines is made to be risen to from 92.11% 93.61%.Bisguanides and urea these solids are intercepted by filter press and are burned, the processing pressure of the three wastes, benzene are reduced Amine consumption has dropped about 20kg/t.

And the device used is fairly simple, and flow is shorter, and the fixed assets investment cost of processing is smaller.

Description of the drawings

Fig. 1 is a kind of device cross-section structure and process flow diagram of the utility model；

In figure, 1- centrifuges；2- water tanks；3- membrane filters；4- addition reaction kettles；5-PH is counted；6- reacting product outlets.

Specific implementation mode

Phenyl guanidine carbonate recovery device in waste water as shown in Figure 1 has and presses the sequentially connected centrifuge of flow 1, water tank 2, membrane filter 3, addition reaction kettle 4, phenyl guanidine carbonate follow-up equipment；Enter with solid on addition reaction kettle 4 Mouth, hydrochloric acid entrance, reacting product outlet 6.

Water tank bottom has nitrogen bubbling device, and water circulating pump is connected between centrifuge and water tank.Addition reaction kettle 4 separately has PH counts 5 sockets, and hydrochloric acid inlet is connected with control valve, PH meters 5 and control valve chain control.

Claims (4)

1. phenyl guanidine carbonate recovery device in a kind of waste water, it is characterised in that：With by the sequentially connected centrifugation of flow Machine, water tank, membrane filter, addition reaction kettle, phenyl guanidine carbonate follow-up equipment；There is solid inlet, hydrochloric acid on addition kettle Entrance, reacting product outlet.

2. phenyl guanidine carbonate recovery device in waste water as described in claim 1, it is characterised in that：Water tank bottom has nitrogen Enraged bulb apparatus.

3. phenyl guanidine carbonate recovery device in waste water as described in claim 1, it is characterised in that：Centrifuge and water tank Between be connected with water circulating pump.

4. phenyl guanidine carbonate recovery device in waste water as described in claim 1, it is characterised in that：Addition reaction kettle is another There is PH to count socket, hydrochloric acid inlet is connected with control valve, PH meters and control valve chain control.