CN1225511C - Phthalocyanine dye deep processing technology - Google Patents
Phthalocyanine dye deep processing technology Download PDFInfo
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- CN1225511C CN1225511C CN 03178312 CN03178312A CN1225511C CN 1225511 C CN1225511 C CN 1225511C CN 03178312 CN03178312 CN 03178312 CN 03178312 A CN03178312 A CN 03178312A CN 1225511 C CN1225511 C CN 1225511C
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Abstract
The present invention discloses a deep processing technology for phthalocyanine pigment. A copper phthalocyanine technology comprises the steps of transforming by ball milling, impurity removing, iron removing, acid treating, filter pressing, rinsing, alkali treating, filter pressing, rinsing, baking, pulverizing, etc. A pigment green technology has the steps of chlorine introducing for reaction, acid treating, alkali treating, rinsing, baking, pulverizing and choice product obtaining, wherein after spongy copper in mother liquid treated by acid is extracted, the mother liquid treated by alkali and rinsing water can be cycled, the problem of large sewage amount in pigment industry for a long time is solved, the product yield is improved by 1.2%, the water consumption is reduced by 98%, the acid consumption is reduced by 74.32%, the alkali consumption is reduced by 80%, each ton products has more than 1800 Yuan of the income, and the present invention perfectly achieves the effects of pollution reduction, quality improvement and benefit creation.
Description
One, technical field: the present invention relates to a kind of phthalocyanine green pigment deep processing technology.
Two, background technology: phthualocyanine pigment is made up of four pyrrole network nuclears, it generally is the organic complex that contains atoms metals such as copper, different blueness of many coloured light or veridian are arranged, and the light fastness of height is arranged, can be used for the dyeing of plastics, printing ink, paint, cotton, silk, paper etc. and the toning of ferric oxide.At present, phthalocyanine blue is by Tetra hydro Phthalic anhydride and cuprous chloride, urea, and crude product is made in heating in the presence of catalyzer, phthalocyanine green by the elaboration copper phthalocyanine by chlorine reaction, acid-alkali treatment, rinsing, oven dry, pulverize elaboration, the sewage discharge of this technology is many.The traditional deep processing technology of phthalocyanine blue pigment be with crude product through ball milling transition, acid treatment, press filtration rinsing, alkaline purification, press filtration rinsing, oven dry, pulverize finished product.The deficiency of this technology is because the Ordinary Wear and Tear of ball milling makes the iron level height, and acid and alkali consumption is big, and sewage discharge is many, causes serious environmental to pollute.
Three, summary of the invention: technical problem to be solved by this invention provides a kind of phthalocyanine green pigment deep processing technology that reduces large amount of sewage discharging, environmental protection.
For solving the problems of the technologies described above, phthalocyanine green deep processing technology of the present invention is:
A, with massfraction be 8 to 9 times of restored acid aqueous mother liquor of copper phthalocyanine crude product overstriking product quality of 60% be made into massfraction be 10% hydrochloric acid or sulphuric acid soln at 80 ℃---100 ℃ of reactions 6---press filtration after 8 hours, oven dry to make massfraction be 95% copper phthalocyanine elaboration;
Mother liquor after B, the press filtration is delivered to acid mother liquid reuse groove No. 1 after adding capacity iron powder reducing+divalent cupric ion filtration extraction copper sponge;
C, with the logical chlorine reaction of copper phthalocyanine elaboration 6 hours, acid mother liquid reuse groove is delivered in attached product acid No. 2;
D, with attached product acid and restored acid aqueous mother liquor make that massfraction is 4.5%, quality is product 8---9 times solution and the product behind the introduce chlorine gas to make reaction are at 80 ℃---100 ℃ of reactions 6---, and acid mother liquid reuse groove is delivered in press filtration after 8 hours, filtrate No. 2;
Use rinse cycle water rinse 6 hours after E, the press filtration, rinse water are collected circulating water pool;
The alkaline mother liquor that product behind F, the acid-respons and this product quality are 8 to 9 times add caustic soda make massfraction be 2.5% solution at 80 ℃---100 ℃ of reactions 6---alkaline mother liquor reuse groove is delivered in press filtration after 8 hours, filtrate;
Use rinse cycle water rinse 8 hours after G, the press filtration, rinse water are collected circulating water pool;
Product drying after H, the rinsing, pulverize finished product.
The required equipment of above-mentioned technology all is conventional chemical industry equipment, and desired raw material also all is the industrial raw material that is easy to get.
Because technique scheme after acid treatment, is carried out the extraction of copper sponge, guaranteed the quality product that Recycling Mother Solution is used.The continuous recovery of mother liquor is used and can be reached mother liquor " zero " discharging.Rinse water can be recycled, and have solved the many difficult problems of pigment industry sewage for a long time.Needing 500 tons of water to reduce to product per ton by former product per ton only needs below 10 tons.
Adopt technique scheme, (1), can improve product yield 1.2%; (2), reduce water 98%; (3) copper sponge of Ti Quing is increased income 200 yuan; (4), the hydrochloric acid consumption is reduced to 0.95 ton by former 3.7 tons, minimizing consumption 74.32%; Reduce alkali consumption 80%.Surplus above-mentioned 4 comprehensive wound benefits 1800 yuan.Reached fully to reduce and polluted, improved quality, the effect of create beneficial result.
Four, description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Five, embodiment:
The embodiment of phthalocyanine green deep processing technology of the present invention is described according to Fig. 1 below.
Embodiment 1
A, with massfraction 60% copper phthalocyanine crude product 10kg, adding hydrochloric acid with restored acid aqueous mother liquor 80kg, to make massfraction be that 10% solution was warming up to 100 ℃ of reactions after 6 hours in reactor, and it is 95% copper phthalocyanine elaboration that massfraction is made in press filtration again, oven dry;
Mother liquor after B, the press filtration is delivered to acid mother liquid reuse groove No. 1 after adding capacity iron powder reducing+divalent cupric ion filtration extraction copper sponge;
C, with the logical chlorine reaction of copper phthalocyanine elaboration 6 hours, acid mother liquid reuse groove is delivered in attached product acid No. 2;
D, attached product acid and restored acid aqueous mother liquor are made massfraction is that 4.5% solution 80kg and the product behind the introduce chlorine gas to make reaction were warming up to 100 ℃ of afterreactions 6 hours in reactor, imports the pressure filter press filtration again, and filtrate is delivered to acid mother liquid reuse groove No. 2;
Use rinse cycle water rinse 6 hours after E, the press filtration, rinse water are collected circulating water pool;
F, adding caustic soda with the 80kg alkaline mother liquor, to make massfraction be 2.5% solution, was warming up to 80 ℃ of afterreactions 8 hours in reactor with product behind the acid-respons, imports the pressure filter press filtration again, and filtrate is delivered to alkaline mother liquor reuse groove;
Product after G, the press filtration is used rinse cycle water rinse 8 hours, and rinse water are collected circulating water pool;
Product drying after H, the rinsing, pulverize finished product.
Embodiment 2
A, with massfraction 60% copper phthalocyanine crude product 10kg, adding hydrochloric acid with restored acid aqueous mother liquor 90kg, to make massfraction be that 10% solution was warming up to 80 ℃ of reactions after 8 hours in reactor, and it is 95% copper phthalocyanine elaboration that massfraction is made in press filtration again, oven dry;
Mother liquor after B, the press filtration is delivered to acid mother liquid reuse groove No. 1 after adding capacity iron powder reducing+divalent cupric ion filtration extraction copper sponge;
C, with the logical chlorine reaction of copper phthalocyanine elaboration 6 hours, acid mother liquid reuse groove is delivered in attached product acid No. 2;
D, attached product acid and restored acid aqueous mother liquor are made massfraction is that 4.5% solution 90kg and the product behind the introduce chlorine gas to make reaction were warming up to 80 ℃ of afterreactions 8 hours in reactor, imports the pressure filter press filtration again, and filtrate is delivered to acid mother liquid reuse groove No. 2;
Use rinse cycle water rinse 6 hours after E, the press filtration, rinse water are collected circulating water pool;
F, adding caustic soda with the 90kg alkaline mother liquor, to make massfraction be 2.5% solution, was warming up to 100 ℃ of afterreactions 8 hours in reactor with product behind the acid-respons, imports the pressure filter press filtration again, and filtrate is delivered to alkaline mother liquor reuse groove;
Product after G, the press filtration is used rinse cycle water rinse 8 hours, and rinse water are collected circulating water pool;
Product drying after H, the rinsing, pulverize finished product.
Embodiment 3
A, with massfraction 60% copper phthalocyanine crude product 10kg, adding sulfuric acid with restored acid aqueous mother liquor 80kg, to make massfraction be that 10% solution was warming up to 90 ℃ of reactions after 7 hours in reactor, and it is 95% copper phthalocyanine elaboration that massfraction is made in press filtration again, oven dry;
Mother liquor after B, the press filtration is delivered to acid mother liquid reuse groove No. 1 after adding capacity iron powder reducing+divalent cupric ion filtration extraction copper sponge;
C, with the logical chlorine reaction of copper phthalocyanine elaboration 6 hours, acid mother liquid reuse groove is delivered in attached product acid No. 2;
D, attached product acid and restored acid aqueous mother liquor are made massfraction is that 4.5% solution 85kg and the product behind the introduce chlorine gas to make reaction were warming up to 90 ℃ of afterreactions 7 hours in reactor, imports the pressure filter press filtration again, and filtrate is delivered to acid mother liquid reuse groove No. 2;
Use rinse cycle water rinse 6 hours after E, the press filtration, rinse water are collected circulating water pool;
F, adding caustic soda with the 80kg alkaline mother liquor, to make massfraction be 2.5% solution, was warming up to 90 ℃ of afterreactions 7 hours in reactor with product behind the acid-respons, imports the pressure filter press filtration again, and filtrate is delivered to alkaline mother liquor reuse groove;
Product after G, the press filtration is used rinse cycle water rinse 8 hours, and rinse water are collected circulating water pool;
Product drying after H, the rinsing, pulverize finished product.
Claims (1)
1, a kind of phthalocyanine green pigment deep processing technology, step is:
A, with massfraction be 8 to 9 times of restored acid aqueous mother liquor of copper phthalocyanine crude product overstriking product quality of 60% be made into massfraction be 10% hydrochloric acid or sulphuric acid soln 80 ℃-100 ℃ reaction press filtrations after 6-8 hour, it is 95% copper phthalocyanine elaboration that massfraction is made in oven dry;
Mother liquor after B, the press filtration is delivered to acid mother liquid reuse groove No. 1 after adding capacity iron powder reducing+divalent cupric ion filtration extraction copper sponge;
C, with the logical chlorine reaction of copper phthalocyanine elaboration 6 hours, acid mother liquid reuse groove is delivered in attached product acid No. 2;
D, with attached product acid and restored acid aqueous mother liquor make that massfraction is 4.5%, quality be product 8-9 solution doubly with the product behind the introduce chlorine gas to make reaction 80 ℃-100 ℃ react 6-8 hour after press filtrations, filtrate is delivered to acid mother liquid reuse groove No. 2;
Use rinse cycle water rinse 6 hours after E, the press filtration, rinse water are collected circulating water pool;
The alkaline mother liquor that product behind F, the acid-respons and this product quality are 8 to 9 times add caustic soda make massfraction be 2.5% solution 80 ℃-100 ℃ reaction press filtrations after 6-8 hour, filtrate is delivered to alkaline mother liquor reuse groove;
Use rinse cycle water rinse 8 hours after G, the press filtration, rinse water are collected circulating water pool;
Product drying after H, the rinsing, pulverize finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03178312 CN1225511C (en) | 2003-05-01 | 2003-07-08 | Phthalocyanine dye deep processing technology |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN03124218 | 2003-05-01 | ||
| CN03124218.9 | 2003-05-01 | ||
| CN 03178312 CN1225511C (en) | 2003-05-01 | 2003-07-08 | Phthalocyanine dye deep processing technology |
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| Publication Number | Publication Date |
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| CN1478825A CN1478825A (en) | 2004-03-03 |
| CN1225511C true CN1225511C (en) | 2005-11-02 |
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| CN 03178312 Expired - Fee Related CN1225511C (en) | 2003-05-01 | 2003-07-08 | Phthalocyanine dye deep processing technology |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100427549C (en) * | 2004-11-15 | 2008-10-22 | 东南大学 | Process for removing heavy metals in dye by companion method |
| CN105647225B (en) * | 2014-12-08 | 2017-07-18 | 池州泰阳颜料有限公司 | A kind of preparation method of Phthalocyanine Green G |
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