CN1083418A

CN1083418A - From organic silicon chemical waste residue, reclaim the technology of useful matter

Info

Publication number: CN1083418A
Application number: CN92110582A
Authority: CN
Inventors: 吴玉琨
Original assignee: Individual
Current assignee: Individual
Priority date: 1992-09-01
Filing date: 1992-09-01
Publication date: 1994-03-09

Abstract

The invention provides a kind of processing method that from organic slag waste residue, reclaims useful matter.Its feature is that waste residue is carried out fluid flotation and gravitational segregation, sub-elect silicon monomer and blister copper powder, again sorting postprecipitation material is put into reactor and be carried out to reactant salt with sulfuric acid, resultant of reaction is obtained high purity, high order copper powder through electrolysis, white carbon black is made in the throw out burning after the electrolysis.This method can reclaim the various useful matteies in organic chemical industry's waste residue effectively, and yield is higher simultaneously, is a kind of good method that turns waste into wealth.

Description

Process for recovering useful substances from organic silicon chemical waste residues

The invention provides a process for recovering useful substances from organic silicon chemical waste residues, belonging to the field of chemical industry.

In the production of organic silicon chemical products, methyl silane and phenyl silane, silicon monomer is one of the main raw materials, copper powder or copper chloride is used as a reaction catalyst, and therefore, the waste residue contains a considerable amount of silicon monomer, copper oxide and other inorganic substances. However, the waste residue contains more impurities, and the separation is difficult. At present, only a few enterprises replace part of copper by a reduction method, but the purity of therecovered copper is not high due to more impurity types and difficult separation.

The invention aims to provide a process method for separating and recovering silicon monomers and copper powder with higher purity from organic silicon chemical waste residues and preparing white carbon black.

The technical scheme of the invention is that waste residue from the production of methyl chlorosilane or phenyl chlorosilane is subjected to fluid flotation and gravity separation; placing the sorted precipitate into a reaction kettle, heating to 80-116 ℃, introducing air, and simultaneously keeping the temperature in the reaction kettle within the range of 80-116 ℃; introducing air for 5-10 minutes, adding 25-30% dilute sulfuric acid into the reaction kettle for reaction, stopping heating and introducing air after 2-4 hours, pouring out substances in the reaction kettle, and filtering; the filtrate is put into an electrolytic bath for electrolysis or directly concentrated and crystallized to prepare the copper sulfate. And (3) performing flotation on the filtered precipitate, precipitating the escaped liquid after the fluid flotation, and burning the precipitate.

The fluid flotation is carried out to separate out the silicon monomer because the silicon monomer is angular and has larger water resistance and the copper and the oxide particles of the copper are heavierAnd (3) performing gravity separation, separating silicon monomers from copper and copper chlorides in the waste residues, putting the separated precipitates into a reaction kettle, simultaneously taking a certain amount of precipitates to analyze the content of copper and copper oxides, heating the reaction kettle to enable the internal temperature to reach 80-116 ℃, and introducing air. At this time, copper is oxidized into copper oxide or cuprous oxide. The reaction equationis as follows: . Continuously introducing air and heating, continuously reacting, introducing air for 5-10 min, then pouring 25-30% dilute sulfuric acid into the reaction kettle, continuously introducing air and heating, wherein the reaction equation of the copper oxide and the dilute sulfuric acid is as follows: the amount of the dilute sulfuric acid added is preferably 1.2 times the amount of the sulfuric acid required for the salt formation reaction of all the copper and copper oxides contained in the precipitate charged into the kettle. Adding dilute sulfuric acid to react for 2-4 hr. After the reaction is finished, pouring out substances in the reaction kettle, and filtering to obtain filtrate, namely copper sulfate solution. Putting the filtered copper sulfate into an electrolytic cell for electrolysis, and separating out copper powder at the cathode of the electrolytic cell, wherein the reaction formula is as follows: . Filtering the substances in the reaction kettle, performing fluid floating body flotation on the precipitate, further performing flotation on the silicon monomer in the precipitate, performing precipitation on the escaped liquid after the two times of flotation, and burning the precipitate to prepare the white carbon black.

The process method for extracting useful substances from the chemical waste residues for producing the methyl chlorosilane or the phenyl chlorosilane can effectively extract the useful substances from the organic silicon chemical waste residues, has high yield, the purity of the silicon monomer recovered by the method reaches over 93 percent, and the copper powder obtained by electrolyzing and extracting the silicon monomer after salt forming reaction is high-mesh copper powder with the purity of over 99 percent and the fineness of over 240 meshes. The copper powder is used for organic silicon chemical production, the surface area per unit weight is large, the yield of finished products can be improved, and after separation, the mixture of combustible substances and silicon dioxide in waste residues is used for burning to prepare white carbon black, so that useful substances in the waste residues are extracted as far as possible, and waste is changed into valuable.

Example (b):

1. taking 1 ton of methyl chlorosilane chemical waste residue, firstly carrying out fluid flotation and gravity separation on the waste residue, putting 310Kg of separated precipitate into a reaction kettle, adding water to submerge the material surface, heating to 80 ℃, ventilating the reaction kettle, adding 290Kg of 30 percent dilute sulfuric acid, reacting for 3.5 hours, filtering the material in the reaction kettle, putting the filtered copper sulfate solution into an electrolytic cell for electrolysis, taking 48.5Kg of 240-mesh copper powder from a cathode after electrolysis, then carrying out secondary separation on the filtered precipitate to obtain 24OKg93.5 percent silicon monomer, taking the secondary separated precipitate as fuel, and sucking 96Kg of white carbon black from all flues after combustion.

2. Taking 1 ton of phenyl chlorosilane chemical waste residue, carrying out fluid flotation, putting 450Kg of separated precipitate into a reaction kettle, adding water to submerge the precipitate on the surface of the material, heating to 80 ℃, introducing air, adding 25% dilute sulfuric acid l400Kg, reacting for 4 hours, filtering the reaction substances, putting the filtered copper sulfate solution into an electrolytic cell for electrolysis, and obtaining 310Kg of pure copper powder from a cathode after electrolysis. And sorting the reacted precipitate, using the precipitate as fuel, and obtaining50Kg of white carbon black from the whole flue after combustion.

Claims

1. A process for recovering useful substances from organic silicon chemical waste residues is characterized in that:

(a) carrying out fluid flotation and gravity separation on the waste residues;

(b) putting the precipitate obtained in the step (a) into a reaction kettle, heating to 80-116 ℃, introducing air, and simultaneously keeping the temperature in the reaction kettle between 80 and 116 ℃;

(c) after air is introduced for 5-10 minutes, 25-30% dilute sulfuric acid is added into the reaction kettle for reaction, after 2-4 hours, heating and air introduction are stopped, and substances in the reaction kettle are poured out and filtered;

(d) and (c) putting the filtrate obtained in the step (c) into an electrolytic bath for electrolysis.

2. The process according to claim 1, characterized in that:

(e) subjecting the precipitate filtered in step (c) to flotation.

3. The process according to claim 1 or 2, characterized in that:

(f) and (e) precipitating the escaped liquid obtained in the step (a) and the step (e) after fluid flotation, and burning the precipitate.