CN101519228A - Process for preparing poly-ferric sulfate chloride by oxidation of oxyful - Google Patents
Process for preparing poly-ferric sulfate chloride by oxidation of oxyful Download PDFInfo
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- CN101519228A CN101519228A CN200910068445A CN200910068445A CN101519228A CN 101519228 A CN101519228 A CN 101519228A CN 200910068445 A CN200910068445 A CN 200910068445A CN 200910068445 A CN200910068445 A CN 200910068445A CN 101519228 A CN101519228 A CN 101519228A
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- ferric sulfate
- hydrogen peroxide
- sulfate chloride
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Abstract
The invention discloses a process for preparing poly-ferric sulfate chloride by oxidation of oxyful, which comprises the following steps: iron sulfate heptahydrate is stirred and added into a reaction tank, and industry by-product hydrochloric acid is added into the reaction tank; oxyful containing 30-35 percent of hydrogen peroxide (H2O2) is slowly and uniformly added into the reaction tank; 5 percent of natrium hydroxide (NaOH) solution is slowly and uniformly added into the reaction tank, and a poly-ferric sulfate chloride product which has 8-14 percent of degree of basification is produced; the poly-ferric sulfate chloride product in the reaction tank is put into a curing tank to be cured for 10 days, and the chemical index of the poly-ferric sulfate chloride product is adjusted to a required value. The invention has the advantages of environmentally-friendly and wide raw material source, small investment, quick return, chemical industry environmental protection and zero discharge of industrial waste. In addition, the invention adopts the oxyful for oxidation and is easy and convenient to operate and control.
Description
Technical field
The present invention relates to be the preparation poly-ferric sulfate chloride technology, particularly be the technology for preparing poly-ferric sulfate chloride with hydrogen peroxide oxidation.
Background technology
At present, in the prior art sewage treatment industry, need promptly to utilize this inorganic flocculating agent that the mud in the sewage is condensed, make sludge settling, realize purification sewage with a large amount of inorganic flocculating agents.Above-mentioned inorganic flocculating agent comprises: aluminum salt flocculant and molysite flocculation agent, and there are following defective in aluminum salt flocculant and molysite flocculation agent in sewage treatment process: the water residual aluminum after handling with aluminum salt flocculant, the serious harm that human body is brought and the biological poison of aluminium; Poor with molysite (bodied ferric sulfate, iron trichloride) flocculation agent coagulation effect, product performance are bad.
For overcoming above-mentioned defective, use inorganic polymer flocculant in the prior art, as doing sewage disposal with poly-ferric sulfate chloride.Poly-ferric sulfate chloride is to have the following advantages as water conditioner: the PH scope that 1) is suitable for water quality is wide, and PH all can reach decontamination effect improving in the 4-11 scope.2) use the poly-ferric sulfate chloride treatment agent because this product density is big than aluminium salt, and reacted throw out is tight, sludge quantity obviously is less than aluminium series coagulating agent.3) coagulating is rapid, and settling velocity is fast, and water is clarified easily with mud and separated.4) that the temperature of processed water, turbidity, basicity etc. are changed adaptability is strong for product, 5) price is relatively low honest and clean.This product has bigger commercial market at home.
At present, the technology of prior art for preparing poly-ferric sulfate chloride all be unable to do without oxidation style, and what adopt usually is catalyzer air (oxygen) oxidation style and sodium chlorate oxidation style.
The technology that adopts catalyzer air (oxygen) oxidation style to prepare poly-ferric sulfate chloride comprises:
In the state downhill reaction jar that stirs, add hydrochloric acid pickling waste liquor or industrial by-product hydrochloric acid, add then through calculating 7 good aqueous ferrous sulfates and adding the Sodium Nitrite catalyzer, depress lasting aerating oxygen at 1.0-1.3 standard atmosphere, temperature of reaction is controlled at 90 ± 5 ℃, sustained reaction 4 hours can reach reaction end.The shortcoming that adopts the catalyst oxygen oxidation style to exist is: 1) investment is big, and the equivalent production capacity level needs bigger conversion unit, promptly needs temperature of reaction can reach 90 ± 5 ℃ heating installation, and positive pressure operation requires high to retort; 2) need add catalyzer in system, Sodium Nitrite is a kind of deleterious and the salt of carcinogenic type arranged; 3) long reaction time.
The technology that adopts the sodium chlorate oxidation style to prepare poly-ferric sulfate chloride comprises: add hydrochloric acid pickling waste liquor or industrial by-product hydrochloric acid in the state downhill reaction jar that stirs, add then through calculating 7 good aqueous ferrous sulfates, the sodium chlorate that adds requirement, reaction times 5-20 minute, can reach reaction end.The shortcoming that adopts the sodium chlorate oxidation style to exist is: 1) sodium chlorate is a kind of inorganic salt, produce after the oxidizing reaction sodium-chlor and remaining sodium chlorate will stay in the product systems, product tape has pungent odour, influences quality product.2) pungent odour that has the utmost point to be subjected to unbearably in the reaction process produces, contaminate environment and injury HUMAN HEALTH.3) the equivalent price of sodium chlorate is than hydrogen peroxide height.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned technology, provide a kind of byproduct to make raw material with industry, prepare poly-ferric sulfate chloride technology with easy hydrogen peroxide oxidation, realize easy and simple to handle, reaction times is short, has a kind of technology for preparing poly-ferric sulfate chloride with hydrogen peroxide oxidation of environment-friendly type.
The technical scheme that solves the problems of the technologies described above is: a kind ofly prepare the technology of poly-ferric sulfate chloride with hydrogen peroxide oxidation, the described technology for preparing poly-ferric sulfate chloride with hydrogen peroxide oxidation is carried out as follows: 1.. under the state that stirs with 7 aqueous ferrous sulfate (FeSO
4.7H
2O) add in the retort, and add the industrial by-product hydrochloric acid of hydrochloric acid (HCl) concentration 〉=25%, described 7 aqueous ferrous sulfate (FeSO
4.7H
2O) content 〉=90%; 2.. with hydrogen peroxide (H
2O
2) content is that the hydrogen peroxide of 30-35% slowly evenly adds in the retort of above-mentioned steps described in 1., the retort temperature is controlled to be 50-75 ℃, reaction times is 40-80 minute, and hydrogen peroxide should all add in the time period equably at the 70-80% of total overall reaction time; 3.. with concentration is that 5% sodium hydroxide (NaOH) solution slowly evenly adds in the retort of above-mentioned steps described in 2., generates the poly-ferric sulfate chloride product, and the basicity of this poly-ferric sulfate chloride product is 8%-14%; 4.. with above-mentioned steps 3. the poly-ferric sulfate chloride product in the retort put into the ageing tank slaking 10 days, and the chemical index of poly-ferric sulfate chloride product is adjusted to desirable value.
The invention has the beneficial effects as follows: 7 aqueous ferrous sulfates in the raw materials technology of the present invention utilize byproduct, the salt acid-utilising industry byproduct hydrochloric acid of titanium coatings industry, so raw materials technology of the present invention source is that environmental protection is extensive again.The present invention uses above-mentioned industry byproduct to make, and has less investment, instant effect, can reach the trade waste zero release, high added value, cost be low, and the present invention is the inorganic water purification agent with advantages such as environmental protective chemical industries.
The present invention adopts hydrogen peroxide oxidation, and the technology catalyst-free does not have other ion components to enter system, and its technological operation is easy, and control is easy, and the reaction times is short, and facility investment is few.
Embodiment
Below embodiments of the invention are described in further detail.
The invention provides and a kind ofly prepare the technology of poly-ferric sulfate chloride with hydrogen peroxide oxidation, the described technology for preparing poly-ferric sulfate chloride with hydrogen peroxide oxidation is carried out as follows:
1.. under the state that stirs with 7 aqueous ferrous sulfate (FeSO
4.7H
2O) add in the retort, and add the industrial by-product hydrochloric acid of hydrochloric acid (HCl) concentration 〉=25%, described 7 aqueous ferrous sulfate (FeSO
4.7H
2O) content 〉=90%;
2.. with hydrogen peroxide (H
2O
2) content is that the hydrogen peroxide of 30-35% slowly evenly adds in the retort of above-mentioned steps described in 1., temperature of reaction is controlled to be 50-75 ℃, and the reaction times is 40-80 minute, and hydrogen peroxide should all add in the time period equably at the 70-80% of total overall reaction time;
3.. with concentration is that 5% sodium hydroxide (NaOH) solution slowly evenly adds in the retort of above-mentioned steps described in 2., generates the poly-ferric sulfate chloride product, and the basicity of this poly-ferric sulfate chloride product is 8%-14%;
4.. with above-mentioned steps 3. the poly-ferric sulfate chloride product in the retort put into the ageing tank slaking 10 days, and the chemical index of poly-ferric sulfate chloride product is adjusted to desirable value.
Described retort is corrosion-resistant and has agitator and the reactor of cooling water jecket.
Described 7 aqueous ferrous sulfates are byproducts of titanium coatings industry.
Process using hydrogen peroxide of the present invention prepares poly-ferric sulfate chloride as oxygenant, because the main component of hydrogen peroxide is hydrogen peroxide H
2O
2, hydrogen peroxide H
2O
2Belong to strong oxidizer.Hydrogen peroxide H in acidic solution
2O
2Can be apace with Fe
2+Be oxidized to Fe
3+Its reaction formula is as follows:
2Fe
2++ H
2O
2+ 2H
+=2Fe
3+2H
2O+Q (Q represents the heat that reaction process produces)
From above-mentioned reaction equation, learn, because the final product of this chemical reaction is Fe
3+And water, even final product makes the aqueous solution of poly-ferric sulfate chloride, do not produce any other ionic and pollute, guaranteed the quality of the aqueous products of poly-ferric sulfate chloride.
Above-mentioned 2Fe
2++ H
2O
2+ 2H
+=2Fe
3++ 2H
2It is close to prepare the speed of response of poly-ferric sulfate chloride technology with the sodium chlorate oxidation style in the speed of response of O+Q reaction and the prior art.But when reaction is carried out too violently, will produce a large amount of reaction heat, cause system temperature to raise, cause oxygenant H
2O
2Decompose volatilization fast.In order to improve the utilization ratio of hydrogen peroxide, come controls reaction speed by the adding speed of control hydrogen peroxide, reduce temperature with water coolant simultaneously, avoid the loss of hydrogen peroxide.
In sum, technology of the present invention is to utilize two kinds of other industrial byproducts to make raw material, prepares poly-ferric sulfate chloride by hydrogen peroxide oxidation, overcomes shortcoming of the prior art, after processing treatment of the present invention, produce a kind of outstanding stain water treatment flocculant, improved the added value of original raw material.
Technological process of the present invention more specifically is described below:
One, select following raw material for use:
1) .7 aqueous ferrous sulfate FeSO
4.7H
2O: select the byproduct of titanium coating factory for use, described 7 aqueous ferrous sulfate FeSO
4.7H
2O content 〉=90%; Consumption: 500-600kg;
2) hydrogen peroxide: hydrogen peroxide H
2O
2Content is 30-35%, consumption: 100-175kg;
3) industrial by-product hydrochloric acid: hydrochloric acid HCl content 〉=25%, consumption: 110-180kg;
4) sodium hydroxide NaOH: concentration is the 5% sodium hydroxide NaOH aqueous solution, consumption: 50-100L
The technological operation step is as follows:
1.. under the state that stirs with 7 aqueous ferrous sulfate FeSO
4.7H
2O joins corrosion-resistant and has in the reactor of agitator and cooling water jecket, adds industrial by-product hydrochloric acid again and starts agitator;
2.. slowly evenly add hydrogen peroxide in the retort of above-mentioned step described in 1., the retort temperature is controlled at 50-75 ℃, reacts 40-80 minute.Hydrogen peroxide should all add in the time period equably at the 70-80% of total overall reaction time;
3.. with concentration is that 5% sodium hydroxide NaOH solution slowly evenly adds in the retort of above-mentioned steps described in 2. and generates the poly-ferric sulfate chloride product, and the basicity of this poly-ferric sulfate chloride product is 8%-14%;
4.. with above-mentioned steps 3. the poly-ferric sulfate chloride product in the retort put into the ageing tank slaking 10 days, and the chemical index of poly-ferric sulfate chloride product is adjusted to desirable value.
Described maturing process is: the poly-ferric sulfate chloride aqueous solution unification that will produce is each time put into a big storage tank and is left standstill the storage certain hour.Make different batches product in the slaking storage tank thorough mixing, leave standstill, can make uniform in quality stable like this.By leaving standstill the precipitated removing of process solid impurity, the polymerization hydrolysis reaction carries out more thoroughly, and the total quality of poly-ferric sulfate chloride product is guaranteed.
Claims (3)
1. one kind prepares the technology of poly-ferric sulfate chloride with hydrogen peroxide oxidation, it is characterized in that, the described technology for preparing poly-ferric sulfate chloride with hydrogen peroxide oxidation is carried out as follows:
1.. under the state that stirs with 7 aqueous ferrous sulfate (FeSO
47H
2O) add in the retort, and add the industrial by-product hydrochloric acid of hydrochloric acid (HCl) concentration 〉=25%, described 7 aqueous ferrous sulfate (FeSO
47H
2O) content 〉=90%;
2.. with hydrogen peroxide (H
2O
2) content is that the hydrogen peroxide of 30-35% slowly evenly adds in the retort of above-mentioned steps described in 1., temperature of reaction is controlled to be 50-75 ℃, and the reaction times is 40-80 minute, and hydrogen peroxide should all add in the time period equably at the 70-80% of total overall reaction time;
3.. with concentration is that 5% sodium hydroxide (NaOH) solution slowly evenly adds in the retort of above-mentioned steps described in 2., generates the poly-ferric sulfate chloride product, and the basicity of this poly-ferric sulfate chloride product is 8%-14%;
4.. with above-mentioned steps 3. the poly-ferric sulfate chloride product in the retort put into the ageing tank slaking 10 days, and the chemical index of poly-ferric sulfate chloride product is adjusted to desirable value.
2. want a kind of described in 1 to prepare the technology of poly-ferric sulfate chloride according to right, it is characterized in that described retort is corrosion-resistant and has agitator and the reactor of cooling water jecket with hydrogen peroxide oxidation.
3. want a kind of described in 1 to prepare the technology of poly-ferric sulfate chloride according to right, it is characterized in that described 7 aqueous ferrous sulfates are byproducts of titanium coatings industry with hydrogen peroxide oxidation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100684452A CN101519228B (en) | 2009-04-13 | 2009-04-13 | Process for preparing poly-ferric sulfate chloride by oxidation of oxyful |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100684452A CN101519228B (en) | 2009-04-13 | 2009-04-13 | Process for preparing poly-ferric sulfate chloride by oxidation of oxyful |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101519228A true CN101519228A (en) | 2009-09-02 |
| CN101519228B CN101519228B (en) | 2011-02-02 |
Family
ID=41080052
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100684452A Expired - Fee Related CN101519228B (en) | 2009-04-13 | 2009-04-13 | Process for preparing poly-ferric sulfate chloride by oxidation of oxyful |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466762A (en) * | 2013-08-26 | 2013-12-25 | 苏州富奇诺水治理设备有限公司 | Domestic waste water treatment agent containing activated silica |
| CN104817149A (en) * | 2015-04-24 | 2015-08-05 | 鲁西化工集团股份有限公司 | Method and system for preparing ferric sulfate polychloride from acid pickling waste solution |
| CN106395915A (en) * | 2016-08-31 | 2017-02-15 | 海南宜净环保股份有限公司 | Synthesis method of polymeric ferric sulfate chloride |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295158C (en) * | 2005-05-27 | 2007-01-17 | 彭继增 | Curing production method for poly hydroxy iron sulfate chloride |
-
2009
- 2009-04-13 CN CN2009100684452A patent/CN101519228B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466762A (en) * | 2013-08-26 | 2013-12-25 | 苏州富奇诺水治理设备有限公司 | Domestic waste water treatment agent containing activated silica |
| CN104817149A (en) * | 2015-04-24 | 2015-08-05 | 鲁西化工集团股份有限公司 | Method and system for preparing ferric sulfate polychloride from acid pickling waste solution |
| CN104817149B (en) * | 2015-04-24 | 2017-06-09 | 鲁西化工集团股份有限公司 | A kind of pickle liquor prepares the method and system of poly-ferric sulfate chloride |
| CN106395915A (en) * | 2016-08-31 | 2017-02-15 | 海南宜净环保股份有限公司 | Synthesis method of polymeric ferric sulfate chloride |
| CN106395915B (en) * | 2016-08-31 | 2018-02-23 | 徐州美利圆环保科技有限公司 | A kind of synthetic method of poly-ferric sulfate chloride |
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| Publication number | Publication date |
|---|---|
| CN101519228B (en) | 2011-02-02 |
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