CN109809369A - The method of dye industry Vat Grey BG processing waste residue calcium mud - Google Patents
The method of dye industry Vat Grey BG processing waste residue calcium mud Download PDFInfo
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- CN109809369A CN109809369A CN201711152028.7A CN201711152028A CN109809369A CN 109809369 A CN109809369 A CN 109809369A CN 201711152028 A CN201711152028 A CN 201711152028A CN 109809369 A CN109809369 A CN 109809369A
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- calcium
- filtrate
- potassium sulfate
- potassium
- waste residue
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Abstract
The present invention provides a kind of methods of dye industry Vat Grey BG processing waste residue calcium mud, the waste residue calcium mud is obtained by production Vat Grey BG, waste residue calcium mud is tuned into slurry with industry water, calcium sulfide and filtrate one is obtained by filtration, filtrate one is reacted with hydrochloric acid solution, the mixed solution of chloride containing calcium, potassium chloride and potassium sulfate is obtained, while hydrogen sulfide gas 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 dilute sulfuric acid, reaction generates calcium sulfate, and potassium sulfate and hydrogen chloride are removed by filtration a small amount of impurity, obtain filtrate；Solution is crystallized at different temperature according to the difference of five H 2 O calcium sulphates and potassium sulfate solubility at different temperatures, respectively obtains five H 2 O calcium sulphates and potassium sulfate by main sulfur acid calcium, potassium sulfate and hydrogen chloride in filtrate.
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
The method of industrial reduction ash BG processing waste residue calcium mud.
Background technique
It is useless that the production processes such as the reactive brilliant bule K-NR of dye industry, alkalescence purple, Vat Grey BG, guaiacol generate calcic
Slag closes in waste residue containing calcification at high temperature wherein generally using calcination process containing a large amount of organic substance, inorganic salts etc.
Object is oxidized to sub- calcium, then and after sulfuric acid acidification is recycled with sulfuric acid calcium form.The organic matter in waste residue is sent out at high temperature simultaneously
Raw oxidative decomposition, generates the gases such as sulfur oxide, nitrogen oxide, carbonoxide, hydrochloric acid, water.
Vat Grey BG through condensation, ammonification, oxidation, acylation, is consolidated using phthalic anhydride, ammonium hydroxide, Pyrogentisinic Acid and intermediate RK as raw material
Mutually the reaction such as condensation and the processes such as filtering, drying, spray drying and be made.Intermediate RK by how acid anhydride and ammonium hydroxide are raw material, through ammonification,
Hydrolysis, bob-weight nitrogen, virtueization, cyclization bromination etc. are reacted and the processes such as filtering, dry and are made.RK obtained is produced for Vat Grey BG
Solid phase condensation uses.The filter process of intermediate RK production generates a large amount of waste residue calcium mud.
Detect the waste residue calcium mud that certain station-service above-mentioned technique production Vat Grey BG generates, every 1 ton of production redeem a vow to a god grey BC generate it is useless
Slag calcium mud 989.91kg, Vat Grey BG produce 300 tons per year, then producing waste residue calcium mud per year is 297 tons.Resulting waste residue calcium mud component are as follows:
Calcium chloride 3.44%, calcium sulfide 13.44%, potassium sulfide 3.53%, potassium chloride 3.26%, potassium sulfate 1.67%, water 20.4%,
Organic impurities 50%.
Summary of the invention
Through detecting, the component that certain factory produces the waste residue calcium mud generated during Vat Grey BG per year is as follows: calcium chloride 3.44%, sulphur
Change calcium 13.44%, potassium sulfide 3.53%, potassium chloride 3.26%, potassium sulfate 1.67%, water 20.4%, organic impurities 50%.This is useless
Filter residue of the slag calcium mud from the filter process of intermediate RK production, 1 ton of vat grey BC generation waste residue calcium mud of every production
989.91kg。
The clay standby calcium sulfide of waste residue calcium is used the present invention provides a kind of, the method for five H 2 O calcium sulphates and potassium sulfate is described useless
Slag calcium mud is obtained by production Vat Grey BG, and this method is effectively administered and is utilized the pollution of dye industry waste residue calcium mud, also makes
The compound products for producing various calcics 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 calcium sulfide of waste residue calcium, five water sulphur
The method of sour calcium and potassium sulfate, the waste residue calcium mud are obtained by production Vat Grey BG, and the component of the waste residue calcium mud is as follows: chlorination
Calcium 3.44%, calcium sulfide 13.44%, potassium sulfide 3.53%, potassium chloride 3.26%, potassium sulfate 1.67%, water 20.4% are organic miscellaneous
Matter 50%, this method comprises the following steps:
Step (1) weighs waste residue calcium mud, and waste residue calcium mud is tuned into slurry with industry water, is filtered, and obtains calcium sulfide filter
Cake and filtrate one；It is dry after calcium sulfide filter cake is washed, obtain vulcanization calcium product；
Step (2), the molar content for calculating potassium sulfide in filtrate one, according to mole of potassium sulfide 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 chloride containing calcium, potassium chloride and potassium sulfate, while hydrogen sulfide gas is discharged；
Step (3) filters the mixed solution of the resulting chloride containing calcium of step (2), potassium chloride and potassium sulfate, obtains extremely
A small amount of filter cake impurity and clear filtrate；
Main sulfur acid calcium, potassium sulfate and hydrogen chloride in step (4), filtrate calculate calcium sulfate potassium sulfate in filtrate and contain
Amount is, when according to 0 DEG C, the solubility of potassium sulfate is 4.9g, and the solubility of five H 2 O calcium sulphates is 14.3g, will be subtracted at 0 DEG C of filtrate
Pressure distillation, makes the concentration of potassium sulfate reach supersaturation, and the concentration of five H 2 O calcium sulphates does not reach its saturated concentration, at this point, sulphur
Sour potassium crystallization is precipitated, is filtered, and obtains potassium sulfate and filtrate three；Filtrate three is warming up to 30 DEG C, at this point, the solubility of potassium sulfate
For 40.8g, and the solubility of five H 2 O calcium sulphates is 25g, and filtrate three is evaporated under reduced pressure, the concentration of five H 2 O calcium sulphates is made to reach satiety
With, and the concentration of potassium sulfate does not reach its saturated concentration, at this point, the crystallization of five H 2 O calcium sulphates is precipitated, is filtered, obtains five water sulphur
Sour calcium and filtrate four, filtrate four mixes with next round step (1) resulting slurry and rear recycling.
The invention has the benefit that the clay standby calcium sulfide of waste residue calcium, the method for five H 2 O calcium sulphates and potassium sulfate,
Easy to operate, equipment investment is few, has effectively administered the pollution of dye industry waste residue calcium mud, and realization is turned waste into wealth, and creating can
The economic value of sight.
Specific embodiment
Embodiment
A kind of method of dye industry Vat Grey BG processing waste residue calcium mud, the waste residue calcium mud are production Vat Grey BG institute
, the component of the waste residue calcium mud is as follows: calcium chloride 3.44%, calcium sulfide 13.44%, potassium sulfide 3.53%, potassium chloride
3.26%, potassium sulfate 1.67%, water 20.4%, organic impurities 50%, this method comprises the following steps:
Step (1) weighs 500kg waste residue calcium mud, and waste residue calcium mud is tuned into slurry with industry water, is filtered, obtains sulphur
Change calcium filter cake and filtrate one；It is dry after calcium sulfide filter cake is washed, obtain 67.2kg vulcanization calcium product；
Step (2), the molar content for calculating potassium sulfide in filtrate one, according to mole of potassium sulfide 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 calcium, potassium chloride and potassium sulfate, while hydrogen sulfide gas is discharged；Hydrogen sulfide gas is passed through in lye or recovered
Manufacture hydrosulphuric acid；
Step (3) filters the mixed solution of the resulting chloride containing calcium of step (2), potassium chloride and potassium sulfate, obtains extremely
A small amount of filter cake impurity and clear filtrate, filter cake impurity is buried or burns, and calcium chloride about 17.2kg, chlorine are contained in filtrate
Change potassium about 42.78kg, potassium sulfate about 8.35kg；
Main sulfur acid calcium, potassium sulfate and hydrogen chloride in step (4), filtrate, the content for calculating calcium sulfate in filtrate are
25kg, potassium sulfate content be the content of 60.27kg and hydrogen chloride, when according to 0 DEG C, the solubility of potassium sulfate is 4.9g, and five
The solubility of H 2 O calcium sulphate is 14.3g, by vacuum distillation at 0 DEG C of filtrate to 175L, the concentration of potassium sulfate is made to reach supersaturation, and
The concentration of five H 2 O calcium sulphates does not reach its saturated concentration but, at this point, potassium sulfate crystallization is precipitated, is filtered, obtains 51.7kg sulfuric acid
Potassium and filtrate three；Filtrate three is warming up to 30 DEG C, at this point, the solubility of potassium sulfate is 40.8g, and the solubility of five H 2 O calcium sulphates
For 25g, filtrate three is evaporated under reduced pressure, the concentration of five H 2 O calcium sulphates is made to reach supersaturation, and the concentration of potassium sulfate does not reach it
Saturated concentration obtains five H 2 O calcium sulphates and filtrate four, filtrate four and next round at this point, the crystallization of five H 2 O calcium sulphates is precipitated, is filtered
The resulting slurry mixing of step (1) and rear recycling.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, architectural form cans be flexible and changeable, can be with derivative series product.It only makes several
Simple deduction or replace all shall be regarded as belonging to present invention scope of patent protection determined by the appended claims.
Claims (1)
1. a kind of method of dye industry Vat Grey BG processing waste residue calcium mud, the waste residue calcium mud is production Vat Grey BG gained,
The component of the waste residue calcium mud is as follows: calcium chloride 3.44%, calcium sulfide 13.44%, potassium sulfide 3.53%, potassium chloride 3.26%,
Potassium sulfate 1.67%, water 20.4%, organic impurities 50%, which is characterized in that this method comprises the following steps:
Step (1), weigh waste residue calcium mud, waste residue calcium mud is tuned into slurry with industry water, is filtered, obtain calcium sulfide filter cake and
Filtrate one；It is dry after calcium sulfide filter cake is washed, obtain vulcanization calcium product；
Step (2), calculate filtrate one in potassium sulfide molar content, according to the mole of potassium sulfide and the pure material of hydrogen chloride it
Than being 1: 1.6-2.4, 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 calcium, potassium chloride and potassium sulfate, while hydrogen sulfide gas is discharged；
Step (3) filters the mixed solution of the resulting chloride containing calcium of step (2), potassium chloride and potassium sulfate, obtains extremely a small amount of
Filter cake impurity and clear filtrate；
Main sulfur acid calcium, potassium sulfate and hydrogen chloride in step (4), filtrate, calculating the content of calcium sulfate potassium sulfate in filtrate is,
When according to 0 DEG C, the solubility of potassium sulfate is 4.9g, and the solubility of five H 2 O calcium sulphates is 14.3g, is steamed depressurizing at 0 DEG C of filtrate
It evaporates, the concentration of potassium sulfate is made to reach supersaturation, and the concentration of five H 2 O calcium sulphates does not reach its saturated concentration, at this point, potassium sulfate
Crystallization is precipitated, is filtered, and obtains potassium sulfate and filtrate three；Filtrate three is warming up to 30 DEG C, at this point, the solubility of potassium sulfate is
40.8g, and the solubility of five H 2 O calcium sulphates is 25g, and filtrate three is evaporated under reduced pressure, the concentration of five H 2 O calcium sulphates is made to reach satiety
With, and the concentration of potassium sulfate does not reach its saturated concentration, at this point, the crystallization of five H 2 O calcium sulphates is precipitated, is filtered, obtains five water sulphur
Sour calcium and filtrate four, filtrate four mixes with next round step (1) resulting slurry and rear recycling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711152028.7A CN109809369A (en) | 2017-11-19 | 2017-11-19 | The method of dye industry Vat Grey BG processing waste residue calcium mud |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711152028.7A CN109809369A (en) | 2017-11-19 | 2017-11-19 | The method of dye industry Vat Grey BG processing waste residue calcium mud |
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| CN109809369A true CN109809369A (en) | 2019-05-28 |
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| CN201711152028.7A Pending CN109809369A (en) | 2017-11-19 | 2017-11-19 | The method of dye industry Vat Grey BG processing waste residue calcium mud |
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- 2017-11-19 CN CN201711152028.7A patent/CN109809369A/en active Pending
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190528 |
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| WD01 | Invention patent application deemed withdrawn after publication |