CN213951303U - Organic silicon slurry residue hydrolysis residue and waste contact body resource utilization system - Google Patents

Abstract

The invention belongs to the technical field of utilization of organic silicon waste residues, and particularly relates to a resource utilization system for hydrolyzed residues of organic silicon pulp residues and waste contacts, which comprises an acid attack tank A, wherein the outlet of an acid attack liquid A is connected with a filter press A, filtrate of the filter press A is connected with a reduction tank, and filter residues of the filter press A are connected with an acid attack tank B; an outlet of the acid leaching solution B is connected with a filter press B, filtrate of the filter press B is connected with a reduction tank, and filter residue of the filter press B is connected with a washing tank; the washing liquid outlet is connected with a filter press C, the filtrate of the filter press C is connected with a reduction tank, and the filter residue of the filter press C is connected with an external solid waste incineration system; the reducing tank liquid outlet is connected with a filter press D, the filtrate of the filter press D is connected with the neutralizing and precipitating tank, and the filter residue of the filter press D is sponge copper; and a liquid outlet of the neutralization precipitation tank is collected after passing through a conveying pump of the neutralization precipitation tank. The invention solves the problem of treatment of organic silicon pulp residue and hydrolysis residue containing copper as hazardous waste, and extracts useful copper from waste residue, thereby realizing resource utilization of waste.

Description

Organic silicon slurry residue hydrolysis residue and waste contact body resource utilization system

Technical Field

The invention belongs to the technical field of utilization of organic silicon waste residues, and particularly relates to a resource utilization system for organic silicon pulp residue hydrolysis residues and waste contacts.

Background

Waste contact bodies are generated in the production process of the organic chlorosilane, and mainly fine powder with serious surface pollution, which is continuously discharged by a silicon-copper contact body and a gas-solid separation system deactivated in a fluidized bed reactor. Because the waste contact bodies contain a large amount of silicon and copper, the average particle size of the contact bodies is fine, the activity of the copper powder is high, and the contact bodies are easily oxidized or even burnt when exposed to air. At present, the waste contact bodies are generally treated in a landfill mode, so that a large amount of landfill sites are needed, a large amount of recyclable silicon and copper are wasted, and in addition, the environment is seriously polluted and serious potential safety hazards exist; in the process of synthesizing chlorosilane, chlorosilane liquid substances with high boiling point and extremely complex components are generated, and the substances can carry part of catalyst powder to form a black oily substance to be discharged out of a reaction system, namely slurry residue. The pulp residue is a flammable, easily hydrolyzed and strongly irritant substance, so the pulp residue has to be treated nearby, the treatment means of the pulp residue at present is mainly hydrolysis, namely the pulp residue is hydrolyzed, chlorosilane in the pulp residue reacts with water to generate black solid powder for further treatment, and the hydrolyzed solid powder is the pulp residue hydrolysis residue.

Silicon powder and copper in the waste contact body and the pulp residue hydrolysis slag can be used as raw materials after being recovered, copper belongs to heavy metal, and serious environmental pollution is caused if the copper is not recycled, so that the environment is not protected.

Patent CN101391775 discloses a method for synthesizing trichlorosilane from waste contacts in organochlorosilane production, wherein the waste contacts are used for preparing trichlorosilane, and the waste contacts contain a large amount of copper and a small amount of zinc and other impurities, so that high-purity trichlorosilane cannot be prepared.

Disclosure of Invention

In order to solve the technical problems, the invention provides a recycling system for hydrolyzed residues of organic silicon slurry residues and waste contacts, which can effectively treat the organic silicon slurry residues.

The specific technical scheme is as follows: a resource utilization system for hydrolyzed residues and waste contacts of organic silicon pulp residues comprises an acid leaching tank A, wherein a feeding port is formed in the acid leaching tank A and used for adding pulp residues and acid, an acid leaching solution A outlet is formed in the bottom of the acid leaching tank A, the acid leaching solution A outlet is connected with a filter press A through a conveying pump of the acid leaching tank A, filtrate of the filter press A is connected with a reduction tank, and filter residues of the filter press A are connected with an acid leaching tank B;

the acid leaching tank B is provided with a feeding port for adding acid, the bottom of the acid leaching tank B is provided with an acid leaching liquid B outlet, the acid leaching liquid B outlet is connected with a filter press B through a conveying pump of the acid leaching tank B, filtrate of the filter press B is connected with a reduction tank, and filter residue of the filter press B is connected with a washing tank;

the washing tank is provided with a feeding port for adding washing liquid (water), the bottom of the washing tank is provided with a washing liquid outlet, the washing liquid outlet is connected with a filter press C through a washing tank delivery pump, filtrate of the filter press C is connected with a reduction tank, and filter residue of the filter press C is connected with an external solid waste incineration system;

the reducing tank is provided with a charging hole for adding iron powder, the bottom of the reducing tank is provided with a reducing tank liquid outlet, the reducing tank liquid outlet is connected with a filter press D through a reducing tank conveying pump, filtrate of the filter press D is connected with a neutralization precipitation tank, and filter residue of the filter press D is sponge copper;

the neutralizing and precipitating tank is provided with a feed inlet for adding NaOH solution, the bottom of the neutralizing and precipitating tank is provided with a neutralizing and precipitating tank liquid outlet, and the neutralizing and precipitating tank liquid outlet is collected after passing through a neutralizing and precipitating tank delivery pump;

all be provided with agitating unit on sour groove A, sour groove B, washing tank, reduction tank, the neutralization precipitation tank of invading, agitating unit includes (mixing) shaft, stirring vane and motor, and the (mixing) shaft stretches into to be provided with stirring vane in the cell body, and the (mixing) shaft upper end is provided with the motor.

The method comprises the following steps:

(1) adding the pulp residue hydrolysis residue and the waste contact body into an acid leaching tank A, adding 5-10% hydrochloric acid solution, adding 30-60 kg of sodium chlorate into each ton of dry residue, and fully contacting copper in the waste residue with the acid leaching solution under the stirring of a stirrer for reaction and retention time of 2-5 hours; (2) conveying the solid-liquid mixture in the acid leaching tank A into a filter press A through a conveying pump of the acid leaching tank A for solid-liquid separation, feeding filtrate into a reduction tank, and feeding filter residue into an acid leaching tank B; (3) adding 5-10% hydrochloric acid solution into the acid leaching tank B, adding 30-60 kg of sodium chlorate into each ton of dry residue, and fully contacting copper in the waste residue with the acid leaching solution under the stirring of a stirrer, wherein the reaction retention time is 2-4 hours; (4) conveying the solid-liquid mixture in the acid leaching tank B into a filter press B through a conveying pump of the acid leaching tank B for solid-liquid separation, allowing filtrate to enter a reduction tank, allowing filter residue to enter a washing tank, and performing acid leaching and washing twice to obtain silicon powder with copper content lower than 0.15%;

(5) after being washed by the washing tank, the filter residue is sent to a filter press by a washing tank conveying pump for overnight separation, the filtrate enters a reduction tank, and the filter residue is sent to a solid waste incineration system for incineration treatment;

(6) detecting the copper content in the reduction tank, adding iron powder into the reduction tank, wherein the ratio of the iron powder to the copper is 1.2-1.5:1, and the iron powder and CuCl are₂The solution is subjected to chemical reaction, and copper is replaced to obtain copper and FeCl2 solution; (7) sending the mixed solution into a filter press C through a reduction tank delivery pump for solid-liquid separation to obtain a spongy copper product with the copper content of more than 50%, and sending the filtrate into a neutralization precipitation tank;

(8) NaOH and FeCl are added into a neutralization precipitation tank₂Neutralizing and precipitating the solution and NaOH to obtain iron slag which can be used as a steelmaking raw material, and delivering clear liquid to a sewage treatment station for treatment. Neutralizing the iron slag in the precipitation tank, and reacting sodium hydroxide with ferric chloride to obtain ferric hydroxide precipitate.

Further, the copper content of the solid slag after acid leaching and secondary washing is less than 100mg/L specified by a leaching toxicity identification standard.

Further, the mixing ratio of the pulp residue hydrolysis residues to the waste contact bodies is 2-5: 1.

Has the advantages that:

1. the simple substance copper is dissolved by using a mode of adding sodium chloride by hydrochloric acid.

2. The two-time acid leaching is selected, so that the hydrochloric acid is easy to volatilize, and the sealing requirement of equipment is higher. The two-time acid leaching can better leach copper, mainly adopts waste hydrochloric acid in organic silicon production, uses high-concentration hydrochloric acid with stronger volatility, all production equipment has higher sealing requirements, pressure filter equipment cannot meet the sealing requirements, and hydrochloric acid with too low concentration has poor leaching effect and cannot leach copper well.

3. The raw materials are locally used, hydrochloric acid is generated by utilizing the hydrolysis of the pulp residue, and the efficiency is high, the cost is low. 4. Compared with sulfuric acid leaching, the hydrochloric acid leaching reduces the complexity of wastewater, and the production of organic silicon mainly comprises hydrochloric acid wastewater, and the sulfuric acid leaching needs to purchase sulfuric acid and generate sulfuric acid wastewater. 5. The sponge copper product is produced, and the silicon powder is sold after copper extraction, so that the economic benefit is increased. 6. Changing dangerous wastes into resources and reducing environmental hazards.

After a toxicity leaching experiment, the copper content in the leaching solution is 3.25-33.6mg/l and is less than the minimum standard of dangerous waste of 100mg/l, and solid residues can not be identified as the dangerous waste.

The method adopts hydrochloric acid as an acid leaching solution, adopts a secondary acid leaching mode, adds the acid leaching solution into the acid leaching tank I and the acid leaching tank II, and promotes the reaction of the pulp residue hydrolysis residue and the copper in the waste contact body with the hydrochloric acid to generate CuCl under the action of an additive₂Solution, mixed solution containing CuCl after solid-liquid separation₂The filtrate enters a reduction tank, the solid enters a washing tank for washing, the solid-liquid mixture in the washing tank is subjected to solid-liquid separation by a filter press, the filtrate enters the reduction tank, and the filter residue is sent to a solid waste incineration system for incineration treatment. Adding iron powder and other catalysts into the reduction tank to ensure that the CuCl₂Reducing copper in the solution, filtering, waiting for spongy copper, and precipitating the filtrate in a neutralization precipitation tank to obtain iron mud. The invention solves the problem of treatment of organic silicon pulp residue and hydrolysis residue containing copper as hazardous waste, and extracts useful copper from waste residue, thereby realizing resource utilization of waste.

Drawings

FIG. 1 is a device contact diagram of the present invention;

the acid leaching device comprises a1 acid leaching tank A, a 2 acid leaching tank B, a 3 washing tank, a 4 reduction tank, a 5 neutralization precipitation tank, a6 acid leaching tank A delivery pump, a 7 acid leaching tank B delivery pump, a 8 washing tank delivery pump, a 9 reduction tank delivery pump, a 10 neutralization precipitation tank delivery pump, 11 filter press A, 12 filter press B, 13 filter press C and 14 filter press D.

Detailed Description

The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.

The organic silicon pulp residue hydrolysis residue and waste contact body resource utilization system comprises an acid attack tank A1, wherein a feed inlet is formed in the acid attack tank A1 and used for adding pulp residue and acid, an acid attack liquid A outlet is formed in the bottom of the acid attack tank A1, the acid attack liquid A outlet is connected with a filter press A11 through an acid attack tank A conveying pump 6, filtrate of the filter press A11 is connected with a reduction tank 4, and filter residue of the filter press A6 is connected with an acid attack tank B2;

the acid leaching tank B2 is provided with a feeding port for adding acid, the bottom of the acid leaching tank B2 is provided with an acid leaching liquid B outlet, the acid leaching liquid B outlet is connected with a filter press B12 through an acid leaching tank B conveying pump 7, the filter liquor of the filter press B12 is connected with a reduction tank 4, and the filter residue of the filter press B is connected with a washing tank 3;

a charging opening is formed in the washing tank 3 and used for charging washing liquid (water), a washing liquid outlet is formed in the bottom of the washing tank 3 and connected with a filter press C13 through a washing tank conveying pump 8, filtrate of the filter press C13 is connected with the reduction tank 4, and filter residue of the filter press C is connected with an external solid waste incineration system;

the reduction tank 4 is provided with a charging hole for adding iron powder, the bottom of the reduction tank 4 is provided with a reduction tank liquid outlet, the reduction tank liquid outlet is connected with a filter press D14 through a reduction tank delivery pump 9, the filtrate of the filter press D is connected with a neutralization precipitation tank, and the filter residue of the filter press D is sponge copper;

a feed inlet is arranged on the neutralization precipitation tank 5 and is used for adding NaOH solution, a neutralization precipitation tank liquid outlet is arranged at the bottom of the neutralization precipitation tank 5, and the neutralization precipitation tank liquid outlet is collected after passing through a neutralization precipitation tank conveying pump 10;

all be provided with agitating unit on groove A1, acid invade groove B2, wash tank 3, reduction tank 4, the neutralization precipitation tank 5, agitating unit includes (mixing) shaft, stirring vane and motor, and the (mixing) shaft stretches into to be provided with stirring vane in the cell body, and the (mixing) shaft upper end is provided with the motor.

Example 1

(1) Adding the pulp residue hydrolysis residue and the waste contact body into an acid leaching tank A according to the proportion of 3:1, adding 5 percent (concentration) hydrochloric acid solution, adding 30 kg of sodium chlorate, and fully contacting copper in the waste residue with the acid leaching solution under the stirring of a stirrer, wherein the reaction residence time is 2 hours; (2) conveying the solid-liquid mixture in the acid leaching tank A into a filter press A through a conveying pump of the acid leaching tank A for solid-liquid separation, feeding filtrate into a reduction tank, and feeding filter residue into an acid leaching tank B; (3) adding a 5% hydrochloric acid solution into the acid leaching tank B, adding 30 kg of sodium chlorate into each ton of dry residue, and fully contacting copper in the waste residue with the acid leaching solution under the stirring of a stirrer, wherein the reaction retention time is 2 hours; (4) conveying the solid-liquid mixture in the acid leaching tank B into a filter press B through a conveying pump of the acid leaching tank B for solid-liquid separation, allowing filtrate to enter a reduction tank, allowing filter residue to enter a washing tank, and performing acid leaching and washing twice to obtain silicon powder with copper content lower than 0.15%;

(5) after being washed by the washing tank, the filter residue is sent into a filter press C by a washing tank conveying pump for overnight separation, the filtrate enters a reduction tank, and the filter residue is sent to a solid waste incineration system for incineration treatment;

(6) detecting the copper content in the reduction tank, adding iron powder into the reduction tank, wherein the ratio of the iron powder to the copper is 1.2:1, and the iron powder and the CuCl2 solution undergo a chemical reaction to displace the copper to obtain copper and a FeCl2 solution; (7) sending the mixed solution into a filter press D through a reduction tank delivery pump for solid-liquid separation to obtain a spongy copper product with the copper content of more than 50%, and sending the filtrate into a neutralization precipitation tank;

(8) NaOH is added into the neutralization precipitation tank, FeCl2 solution and the NaOH are neutralized and precipitated to obtain iron slag, the iron slag can be used as a steelmaking raw material, and clear liquid is sent to a sewage treatment station for treatment.

(9) After a toxicity leaching experiment, the copper content in the leaching solution is 3.25-33.6mg/l and is less than the minimum standard of dangerous waste of 100mg/l, and solid residues can not be identified as the dangerous waste.

Example 2

(1) Adding the pulp residue hydrolysis residue and the waste contact body into an acid leaching tank A according to the proportion of 3:1, adding 10 percent (concentration) hydrochloric acid solution, adding 40 kg of sodium chlorate, and fully contacting copper in the waste residue with the acid leaching solution under the stirring of a stirrer, wherein the reaction residence time is 4 hours; (2) conveying the solid-liquid mixture in the acid leaching tank A into a filter press A through a conveying pump of the acid leaching tank A for solid-liquid separation, feeding filtrate into a reduction tank, and feeding filter residue into an acid leaching tank B; (3) adding 8% hydrochloric acid solution into the acid leaching tank B, adding 40 kg of sodium chlorate into each ton of dry residue, and fully contacting copper in the waste residue with the acid leaching solution under the stirring of a stirrer, wherein the reaction retention time is 3 hours; (4) conveying the solid-liquid mixture in the acid leaching tank B into a filter press B through a conveying pump of the acid leaching tank B for solid-liquid separation, allowing filtrate to enter a reduction tank, allowing filter residue to enter a washing tank, and performing acid leaching and washing twice to obtain silicon powder with copper content lower than 0.15%;

(5) after being washed by the washing tank, the filter residue is sent into a filter press C by a washing tank conveying pump for overnight separation, the filtrate enters a reduction tank, and the filter residue is sent to a solid waste incineration system for incineration treatment;

(6) detecting the copper content in the reduction tank, adding iron powder into the reduction tank, wherein the ratio of the iron powder to the copper is 1.3:1, and the iron powder and the CuCl2 solution undergo a chemical reaction to displace the copper to obtain copper and a FeCl2 solution; (7) sending the mixed solution into a filter press D through a reduction tank delivery pump for solid-liquid separation to obtain a spongy copper product with the copper content of more than 50%, and sending the filtrate into a neutralization precipitation tank;

(8) NaOH is added into the neutralization precipitation tank, FeCl2 solution and the NaOH are neutralized and precipitated to obtain iron slag, the iron slag can be used as a steelmaking raw material, and clear liquid is sent to a sewage treatment station for treatment.

(9) After a toxicity leaching experiment, the copper content in the leaching solution is 3.25-33.6mg/l and is less than the minimum standard of dangerous waste of 100mg/l, and solid residues can not be identified as the dangerous waste.

Example 3

(1) Adding the pulp residue hydrolysis residue and the waste contact body into an acid leaching tank A according to the proportion of 3:1, adding 10 percent (concentration) hydrochloric acid solution, adding 60 kg of sodium chlorate, and fully contacting copper in the waste residue with the acid leaching solution under the stirring of a stirrer, wherein the reaction residence time is 5 hours; (2) conveying the solid-liquid mixture in the acid leaching tank A into a filter press A through a conveying pump of the acid leaching tank A for solid-liquid separation, feeding filtrate into a reduction tank, and feeding filter residue into an acid leaching tank B; (3) adding 10% hydrochloric acid solution into the acid leaching tank B, adding 60 kg of sodium chlorate into each ton of dry residue, and fully contacting copper in the waste residue with the acid leaching solution under the stirring of a stirrer, wherein the reaction retention time is 4 hours; (4) conveying the solid-liquid mixture in the acid leaching tank B into a filter press B through a conveying pump of the acid leaching tank B for solid-liquid separation, allowing filtrate to enter a reduction tank, allowing filter residue to enter a washing tank, and performing acid leaching and washing twice to obtain silicon powder with copper content lower than 0.15%;

(5) after being washed by the washing tank, the filter residue is sent into a filter press C by a washing tank conveying pump for overnight separation, the filtrate enters a reduction tank, and the filter residue is sent to a solid waste incineration system for incineration treatment;

(6) detecting the copper content in the reduction tank, adding iron powder into the reduction tank, wherein the ratio of the iron powder to the copper is 1.5:1, and the iron powder and the CuCl2 solution undergo a chemical reaction to displace the copper to obtain copper and a FeCl2 solution; (7) sending the mixed solution into a filter press D through a reduction tank delivery pump for solid-liquid separation to obtain a spongy copper product with the copper content of more than 50%, and sending the filtrate into a neutralization precipitation tank;

(8) NaOH is added into the neutralization precipitation tank, FeCl2 solution and the NaOH are neutralized and precipitated to obtain iron slag, the iron slag can be used as a steelmaking raw material, and clear liquid is sent to a sewage treatment station for treatment.

(9) After a toxicity leaching experiment, the copper content in the leaching solution is 3.25-33.6mg/l and is less than the minimum standard of dangerous waste of 100mg/l, and solid residues can not be identified as the dangerous waste.

Claims (1)

1. The organic silicon pulp residue hydrolysis residue and waste contact body resource utilization system is characterized by comprising an acid attack tank A, wherein a feeding port is arranged on the acid attack tank A and used for adding pulp residue and acid, an acid attack liquid A outlet is arranged at the bottom of the acid attack tank A, the acid attack liquid A outlet is connected with a filter press A through a conveying pump of the acid attack tank A, filtrate of the filter press A is connected with a reduction tank, and filter residue of the filter press A is connected with an acid attack tank B;

the acid leaching tank B is provided with a feeding port for adding acid, the bottom of the acid leaching tank B is provided with an acid leaching liquid B outlet, the acid leaching liquid B outlet is connected with a filter press B through a conveying pump of the acid leaching tank B, filtrate of the filter press B is connected with a reduction tank, and filter residue of the filter press B is connected with a washing tank;

the washing tank is provided with a feeding port for adding washing liquid, the bottom of the washing tank is provided with a washing liquid outlet, the washing liquid outlet is connected with a filter press C through a washing tank delivery pump, filtrate of the filter press C is connected with a reduction tank, and filter residue of the filter press C is connected with an external solid waste incineration system;

the reducing tank is provided with a charging hole for adding iron powder, the bottom of the reducing tank is provided with a reducing tank liquid outlet, the reducing tank liquid outlet is connected with a filter press D through a reducing tank conveying pump, filtrate of the filter press D is connected with a neutralization precipitation tank, and filter residue of the filter press D is sponge copper;

the neutralizing and precipitating tank is provided with a feed inlet for adding NaOH solution, the bottom of the neutralizing and precipitating tank is provided with a neutralizing and precipitating tank liquid outlet, and the neutralizing and precipitating tank liquid outlet is collected after passing through a neutralizing and precipitating tank delivery pump;

all be provided with agitating unit on sour groove A, sour groove B, washing tank, reduction tank, the neutralization precipitation tank of invading, agitating unit includes (mixing) shaft, stirring vane and motor, and the (mixing) shaft stretches into to be provided with stirring vane in the cell body, and the (mixing) shaft upper end is provided with the motor.

Images