CN109835939A - Dyestuff organic chemical industry's industry waste residue copper sludge recovery process - Google Patents
Dyestuff organic chemical industry's industry waste residue copper sludge recovery process Download PDFInfo
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- CN109835939A CN109835939A CN201711208096.0A CN201711208096A CN109835939A CN 109835939 A CN109835939 A CN 109835939A CN 201711208096 A CN201711208096 A CN 201711208096A CN 109835939 A CN109835939 A CN 109835939A
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- filtrate
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- nitrate
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Abstract
The present invention provides dyestuff organic chemical industry's industry waste residue copper sludge recovery process, the waste residue copper sludge is obtained by production Vat Grey BG, waste residue copper sludge is slurred shape object with industry water, cupric iodide and filtrate one is obtained by filtration, filtrate one is reacted with hydrochloric acid solution, the mixed solution of containing copper chloride, sodium chloride and sodium iodate is obtained, while iodate hydrogen is discharged；Mixed solution filtering, obtains extremely a small amount of filter cake impurity and clear filtrate；The air-distillation of clear filtrate elder generation steams the organic impurities of low boiling point, then with excessive nitric acid, reaction generates copper nitrate, and sodium nitrate and hydrogen chloride are removed by filtration a small amount of impurity, obtain filtrate two；Filtrate two is reacted with excess nitric acid calcium removes sodium iodate, is filtered, obtains filtrate three；Mainly contain copper nitrate, sodium nitrate and hydrogen chloride in filtrate three, according to copper nitrate, solution is crystallized at different temperature, respectively obtains copper nitrate, sodium nitrate by the difference of sodium nitrate solubility at different temperatures.
Description
Technical field
The invention belongs to dyestuff organic chemical industry's industry multipurpose use of the three wastes technical fields, and in particular, to be a kind of dyestuff
Organic chemical industry's industry waste residue copper sludge recovery process, the waste residue copper sludge are obtained by production Vat Grey BG.
Background technique
The reactive brilliant bule K-NR of dye industry, alkalescence purple, the production processes such as grey BC, guaiacol of redeeming a vow to a god generate cupric and give up
Slag contains copper chemical combination wherein generally using calcination process containing a large amount of organic substance, inorganic salts etc. at high temperature in waste residue
Object be oxidized to it is cuprous, then and acid iodide acidification after in the form of cupric iodate recycle.The organic matter in waste residue is sent out at high temperature simultaneously
Raw oxidative decomposition, generates the gases such as iodine dioxide, nitrogen oxide, carbon dioxide, hydrochloric acid, water.
Vat grey BC be using phthalic anhydride, ammonium hydroxide, hydroquinone and intermediate RK as raw material, through condensation, ammonification, oxidation, acylation,
The reaction such as solid phase condensation and the processes such as filtering, drying, spray drying and be made.Intermediate RK is by how acid anhydride and ammonium hydroxide are raw material, through ammonia
Change, hydrolysis, bob-weight nitrogen, virtueization, cyclization bromination etc. are reacted and the processes such as filtering, dry and are made.RK obtained is for vat grey BC
Solid phase condensation is produced to use.The filter process of intermediate RK production generates a large amount of waste residue copper sludge.
Detect the waste residue copper sludge that certain station-service above-mentioned technique production vat grey BC is generated, every 1 ton of production redeem a vow to a god grey BC generate it is useless
Slag copper sludge 989.91kg, vat grey BC produce 300 tons per year, then producing waste residue copper sludge per year is 297 tons.Resulting waste residue copper sludge component are as follows:
Copper chloride 3.44%, cupric iodide 13.44%, sodium iodide 3.53%, sodium chloride 3.26%, sodium iodate 1.67%, water 20.4%,
Organic impurities 50%.
Summary of the invention
Through detecting, the component that certain factory produces the waste residue copper sludge generated during vat grey BC per year is as follows: copper chloride 3.44%, iodine
Change copper 13.44%, sodium iodide 3.53%, sodium chloride 3.26%, sodium iodate 1.67%, water 20.4%, organic impurities 50%.This is useless
Filter residue of the slag copper sludge from the filter process of intermediate RK production, 1 ton of vat grey BC generation waste residue copper sludge of every production
989.91kg。
The present invention provides a kind of dyestuff organic chemical industry industry waste residue copper sludge recovery process, the waste residue copper sludge is that production is gone back
Obtained by former ash BG, this method is effectively administered and is utilized the pollution of dye industry waste residue copper sludge, also produces various cuprics
Compound products create considerable economic value, while having well-off social benefit and abundant economic benefit.
To achieve the above object, the technical solution of the present invention is as follows: a kind of use the clay standby cupric iodide of copper waste residues, copper nitrate
With the method for sodium nitrate, the waste residue copper sludge is obtained by production Vat Grey BG, and the component of the waste residue copper sludge is as follows: copper chloride
3.44%, cupric iodide 13.44%, sodium iodide 3.53%, sodium chloride 3.26%, sodium iodate 1.67%, water 20.4%, organic impurities
50%, this method comprises the following steps:
Step (1) weighs waste residue copper sludge, and waste residue copper sludge is slurred shape object with industry water, is filtered, and obtains cupric iodide filter
Cake and filtrate one；It is dry after cupric iodide filter cake is washed, obtain iodate copper products；
Step (2), the molar content for calculating sodium iodide in filtrate one, according to mole of sodium iodide and the pure material of hydrogen chloride
The ratio between amount is 1: 1.6-2.4, and the resulting filtrate one of step (1) is put into corrosion resistant reactor reaction with hydrochloric acid solution, is obtained
The mixed solution of containing copper chloride, sodium chloride and sodium iodate, while iodate hydrogen is discharged；Iodate hydrogen is passed through in lye or passes through
Recycling manufacture hydroiodic acid；
Step (3) filters the mixed solution of the resulting containing copper chloride of step (2), sodium chloride and sodium iodate, obtains extremely
A small amount of filter cake impurity and clear filtrate；
Step (4), the organic impurities that clear filtrate elder generation air-distillation obtained by step (3) is steamed to low boiling point, it is remaining
Three kinds of sodium iodate, sodium chloride and copper chloride substances are mainly contained in solution；
Step (5): the sum of sodium chloride and the molar content of copper chloride in surplus solution are calculated, and according to the molar content
The sum of excessive dust technology is added, reaction generates copper nitrate, sodium nitrate and hydrogen chloride, a small amount of impurity is removed by filtration, obtains
Filtrate two；
Mainly contain copper nitrate, sodium nitrate, sodium iodate and hydrogen chloride in step (6), filtrate two, calculate the content of sodium iodate,
And calcium nitrate is added, and precipitate iodate ion and calcium binding at calcium iodate, and generate sodium nitrate, filtering reacting liquid,
Obtain acid iodide calcium precipitate and filtrate three；Sodium nitrate, copper nitrate and hydrogen chloride are mainly contained in filtrate three
Step (7), calculate filtrate three in copper nitrate, sodium nitrate and hydrogen chloride content, when according to 20 DEG C, copper nitrate it is molten
Xie Du is 125g, and the solubility of sodium nitrate is 87.6g, will be evaporated under reduced pressure at 2 20 DEG C of filtrate, reached the concentration of sodium nitrate
Saturation, and the concentration of copper nitrate does not reach its saturated concentration, at this point, sodium nitrate crystallization is precipitated, is filtered, obtain sodium nitrate and
Filtrate four；Filtrate four is cooled to 0 DEG C, at this point, the solubility of copper nitrate is 83.5g, the solubility of sodium nitrate is 73g, will be filtered
Liquid four is evaporated under reduced pressure, and the concentration of copper nitrate is made to reach supersaturation, and the concentration of sodium nitrate does not reach its saturated concentration, at this point,
Copper nitrate crystallization is precipitated, is filtered, and obtains copper nitrate and filtrate five, and filtrate five and next round step (1) resulting slurry are mixed
It is reused after merging.
The iodate hydrogen of step (2) discharge is passed through in lye or recovered manufacture hydroiodic acid.
The filter cake impurity that step (3) obtains is buried or burns.
Dyestuff organic chemical industry industry waste residue copper sludge recovery process of the present invention, chemical equation are as follows:
Na2S+2HCl====2NaCl+H2S
CuCl2+2HNO3====Cu (NO3) 2+2HCl
NaCl+HNO3====NaNO3+HCl
Na2SO4+Ca (NO3) 2====2NaNO3+CaSO4 ↓
The invention has the benefit that the dyestuff organic chemical industry industry waste residue copper sludge recovery process, easy to operate, equipment
Small investment has effectively administered the pollution of dye industry waste residue copper sludge, and realization is turned waste into wealth, and creates considerable economic value.
Specific embodiment
Embodiment
A kind of dyestuff organic chemical industry industry waste residue copper sludge recovery process, the waste residue copper sludge are production Vat Grey BG gained,
The component of the waste residue copper sludge is as follows: copper chloride 3.44%, cupric iodide 13.44%, sodium iodide 3.53%, sodium chloride 3.26%,
Sodium iodate 1.67%, water 20.4%, organic impurities 50%, this method comprises the following steps:
Step (1) weighs 500kg waste residue copper sludge, and waste residue copper sludge is slurred shape object with industry water, is filtered, obtains iodine
Change copper filter cake and filtrate one；It is dry after cupric iodide filter cake is washed, obtain 67.2kg iodate copper products；
Step (2), the molar content for calculating sodium iodide in filtrate one, according to mole of sodium iodide and the pure material of hydrogen chloride
The ratio between amount is 1: 2.4, and the resulting filtrate one of step (1) is put into corrosion resistant reactor reaction with hydrochloric acid solution, is obtained containing chlorine
Change the mixed solution of copper, sodium chloride and sodium iodate, while iodate hydrogen is discharged；Iodate hydrogen is passed through in lye or recovered
Manufacture hydroiodic acid；
Step (3) filters the mixed solution of the resulting containing copper chloride of step (2), sodium chloride and sodium iodate, obtains extremely
A small amount of filter cake impurity and clear filtrate, filter cake impurity is buried or burns, and copper chloride about 17.2kg, chlorine are contained in filtrate
Change sodium about 42.78kg, sodium iodate about 8.35kg；
Step (4), the organic impurities that clear filtrate elder generation air-distillation obtained by step (3) is steamed to low boiling point, it is remaining
Three kinds of sodium iodate, sodium chloride and copper chloride substances are mainly contained in solution；
Step (5): the sum of sodium chloride and the molar content of copper chloride in surplus solution are calculated, and according to the molar content
The sum of excessive dust technology is added, reaction generates copper nitrate, sodium nitrate and hydrogen chloride, a small amount of impurity is removed by filtration, obtains
Filtrate two；
Mainly contain copper nitrate, sodium nitrate, sodium iodate and hydrogen chloride in step (6), filtrate two, calculate the content of sodium iodate,
And calcium nitrate is added, and precipitate iodate ion and calcium binding at calcium iodate, and generate sodium nitrate, filtering reacting liquid,
Obtain acid iodide calcium precipitate and filtrate three；Sodium nitrate, copper nitrate and hydrogen chloride are mainly contained in filtrate three
The content about 19kg of copper nitrate, the content of sodium nitrate are about 72.1kg in step (7), calculating filtrate three, according to 20
DEG C when, the solubility of copper nitrate is 125g, and the solubility of sodium nitrate is 87.6g, will be evaporated under reduced pressure at 2 20 DEG C of filtrate, makes nitric acid
The concentration of sodium reaches supersaturation, and the concentration of copper nitrate does not reach its saturated concentration, at this point, copper nitrate sodium partial crystallization goes out, passes through
Filter, obtains sodium nitrate and filtrate four；Filtrate four is cooled to 0 DEG C, at this point, the solubility of copper nitrate be 83.5g, sodium nitrate it is molten
Xie Du is 73g, and filtrate four is evaporated under reduced pressure, and the concentration of copper nitrate is made to reach supersaturation, and the concentration of sodium nitrate does not reach it
Saturated concentration obtains copper nitrate and filtrate five at this point, copper nitrate crystallization is precipitated, is filtered, filtrate five and next round step (1)
Resulting slurry mixing and rear recycling.
Claims (1)
1. a kind of dyestuff organic chemical industry industry waste residue copper sludge recovery process, the waste residue copper sludge is institute obtained by production Vat Grey BG
The component for stating waste residue copper sludge is as follows: copper chloride 3.44%, cupric iodide 13.44%, sodium iodide 3.53%, sodium chloride 3.26%, iodine
Sour sodium 1.67%, water 20.4%, organic impurities 50%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711208096.0A CN109835939A (en) | 2017-11-27 | 2017-11-27 | Dyestuff organic chemical industry's industry waste residue copper sludge recovery process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711208096.0A CN109835939A (en) | 2017-11-27 | 2017-11-27 | Dyestuff organic chemical industry's industry waste residue copper sludge recovery process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109835939A true CN109835939A (en) | 2019-06-04 |
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ID=66880379
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711208096.0A Pending CN109835939A (en) | 2017-11-27 | 2017-11-27 | Dyestuff organic chemical industry's industry waste residue copper sludge recovery process |
Country Status (1)
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2017
- 2017-11-27 CN CN201711208096.0A patent/CN109835939A/en active Pending
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Application publication date: 20190604 |