CN103275517B - Method for effectively recovering grinding medium in pigmentation process - Google Patents
Method for effectively recovering grinding medium in pigmentation process Download PDFInfo
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- CN103275517B CN103275517B CN201310199817.1A CN201310199817A CN103275517B CN 103275517 B CN103275517 B CN 103275517B CN 201310199817 A CN201310199817 A CN 201310199817A CN 103275517 B CN103275517 B CN 103275517B
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- pigment
- inorganic salt
- organic solvent
- grinding medium
- efficient recovery
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- 238000000034 method Methods 0.000 title claims abstract description 47
- 238000000227 grinding Methods 0.000 title claims abstract description 28
- 230000019612 pigmentation Effects 0.000 title abstract 2
- 239000000049 pigment Substances 0.000 claims abstract description 81
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 39
- 239000000047 product Substances 0.000 claims abstract description 33
- 239000003960 organic solvent Substances 0.000 claims abstract description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012047 saturated solution Substances 0.000 claims abstract description 16
- 239000002351 wastewater Substances 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims abstract description 7
- 238000004065 wastewater treatment Methods 0.000 claims abstract description 7
- 239000012065 filter cake Substances 0.000 claims abstract description 6
- 239000012266 salt solution Substances 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- 230000000485 pigmenting effect Effects 0.000 claims description 16
- 238000011084 recovery Methods 0.000 claims description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 238000011026 diafiltration Methods 0.000 claims description 5
- 235000019239 indanthrene blue RS Nutrition 0.000 claims description 5
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000013517 stratification Methods 0.000 claims description 5
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical group [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 claims description 4
- PPSZHCXTGRHULJ-UHFFFAOYSA-N dioxazine Chemical compound O1ON=CC=C1 PPSZHCXTGRHULJ-UHFFFAOYSA-N 0.000 claims description 4
- -1 isoindoline ketone Chemical class 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 4
- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical class C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 4
- 239000012043 crude product Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 238000009835 boiling Methods 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 235000019600 saltiness Nutrition 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a method for effectively recovering a grinding medium in a pigmentation process, which is characterized by comprising the following steps: adding a pigment crude product, inorganic salt and organic solvent into a kneader or ball grinder, grinding at 30-100 DEG C for 2-50 hours, throwing the ground materials into clear water, and dissolving while heating to normal temperature-80 DEG C, thus obtaining an inorganic salt saturated solution; standing, stratifying to separate out a solvent layer, dewatering for later use, and filtering a water layer; performing multi-effect concentration on the salt solution, crystallizing, filtering, drying, and pulverizing for later use; throwing filter cakes into a 1-3% hydrochloric acid solution, performing acid boiling at 50-100 DEG C for 1-3 hours, filtering, washing, and drying to obtain a pigment finished product; and directly feeding the filtering and washing waste water into a waste water treatment device, treating to reach the standards, and then discharging. According to the invention, the method is simple in process and favorable in treatment effect; and the COD (chemical oxygen demand) and the salt content in the production waste water can be greatly reduced, thus reducing the biochemical treatment pressure of the waste water.
Description
Technical field
The present invention relates to chemical field, particularly relate to a kind of method of efficient recovery grinding medium in pigmenting process.
Background technology
Pigment dyestuff generally with minuteness particle fractions distribution in coloring medium, the crystal formation of pigment particles, shape, the physical factor such as size and condition of surface all can affect the reflection of light, absorption and scattering, thus affect coloured light, tinting strength, opacifying power and dispersiveness, also can impact performances such as its fast light, heat-resisting, weather simultaneously.
Poor by the crude pigment product crystal stability of chemosynthesis, add that crude product particle is large, thus, tinting strength is low, should not commercial pigments be used as, pigmenting (commercialization) process must be carried out, reduce its globule size, and make it be converted into stable performance, strong coloring force, the stable state crystal of bright in color light.
Pigmenting generally divides acid-solublely analyses method and polishing.Acid-soluble method (US4317908, US4804417) of analysing crude pigment product is dissolved or is partially dissolved in the vitriol oil, then pour in large water gaging, it is made to separate out with fine crystals, stable crystal formation is translated into again through solvent treatment, improve crystal surface morphology simultaneously, the pigment finished product of excellent performance can be obtained.Acid-solublely analyse the sulfuric acid producing large volume low-concentration in method process, wastewater treatment difficulty, cost are high, therefore seldom adopt.Polishing (US6517630B1, US20100101456A1) is ground together with inorganic salt and organic solvent at crude pigment product, boils by acid, directly can obtain the pigment finished product of excellent performance.Polishing needs to add a large amount of inorganic salt (usual 5-10 is doubly to crude pigment product) grinding aid and organic solvent (1-2 is doubly to crude pigment product), and brine waste easily causes microorganism wall to break, thus has a strong impact on wastewater biochemical treatment effect.
Summary of the invention
The object of this invention is to provide a kind of method of efficient recovery grinding medium in pigmenting process.
The technical solution used in the present invention is:
A kind of method of efficient recovery grinding medium in pigmenting process, comprise the steps: crude pigment product, inorganic salt, organic solvent adds in kneader or ball mill, 2-50h is ground at the temperature of 30-100 DEG C, abrasive is dropped in clear water and be heated to normal temperature-80 DEG C dissolving, be configured to the saturated solution of inorganic salt, stratification, solvent layer is separated, apply mechanically after dehydration, water layer filters, salts solution is through Multi-effect concentration, crystallization is filtered, apply mechanically after drying and crushing, filter cake drops in 1-3% hydrochloric acid soln, at the temperature of 50-100 DEG C, 1-3h is boiled in acid, wash after filtration again, dry pigment finished product, diafiltration waste water directly enters wastewater treatment equipment and processes, rear discharge up to standard.
The mass ratio of described crude pigment product, inorganic salt, organic solvent is 1:(5-10): (1-2).
The quality of described hydrochloric acid is 5-30 times of crude pigment product quality.
Described crude pigment product comprises phthalocyanine pigment, dioxazine pigment, Isosorbide-5-Nitrae-diketopyrrolo-pyrrole pigment, condensed ring ketone pigment, isoindoline ketone pigment, quinophthalone class pigment.
Described phthalocyanine pigment is phthalocyanine blue 15, and described dioxazine pigment is pigment Violet 23, described 1,4-diketopyrrolo-pyrrole pigment is Pigment red 254, described condensed ring ketone pigment is pigment blue 60, and described isoindoline ketone pigment is Pigment Yellow 73 110, and described quinophthalone class pigment is pigment yellow 13 8.
Described inorganic salt are Calcium Chloride Powder Anhydrous, sodium-chlor or anhydrous sodium sulphate.
Described organic solvent is water insoluble and grinds the organic solvent of inorganic salt solution used, and the near saturated solution of density and grinding inorganic salt used not etc., can not produce obvious layering.
Described organic solvent density is less than the near saturated solution grinding inorganic salt used.
Described organic solvent is benzene, toluene or dimethylbenzene.
Advantage of the present invention is: this technique is simple, and treatment effect is good, greatly can reduce the COD in factory effluent and saltiness, thus alleviate wastewater biochemical processing pressure.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Fig. 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1
As shown in Figure 1, the method of a kind of efficient recovery grinding medium in pigmenting process of the present invention, comprise the steps: crude pigment product, inorganic salt, organic solvent adds in kneader or ball mill, crude pigment product, inorganic salt, the mass ratio of organic solvent is 1:5:1, 40h is ground at the temperature of 30 DEG C, abrasive is dropped in clear water and be heated to 70 DEG C of dissolvings, be configured to the saturated solution of inorganic salt, stratification, solvent layer is separated, apply mechanically after dehydration, water layer filters, salts solution is through Multi-effect concentration, crystallization is filtered, apply mechanically after drying and crushing, filter cake drops in 3% hydrochloric acid soln, the quality of hydrochloric acid is 5 times of crude pigment product quality, at the temperature of 50 DEG C, 3h is boiled in acid, wash after filtration again, dry pigment finished product, diafiltration waste water directly enters wastewater treatment equipment and processes, rear discharge up to standard.。
Described crude pigment product comprises phthalocyanine blue 15, pigment violet 19, Pigment red 254, pigment blue 60, Pigment Yellow 73 110, pigment yellow 13 8.
Described inorganic salt are Calcium Chloride Powder Anhydrous.
Described organic solvent is water insoluble and grinds the organic solvent of inorganic salt solution used, the near saturated solution of density and grinding inorganic salt used not etc., can not produce obvious layering, optimum, machine solvent density is less than the near saturated solution grinding inorganic salt used, as benzene.
Embodiment 2
As shown in Figure 1, the method of a kind of efficient recovery grinding medium in pigmenting process of the present invention, comprise the steps: crude pigment product, inorganic salt, organic solvent adds in kneader or ball mill, crude pigment product, inorganic salt, the mass ratio of organic solvent is 1:10:2, 20h is ground at the temperature of 50 DEG C, abrasive is dropped in clear water and be heated to 30 DEG C of dissolvings, be configured to the saturated solution of inorganic salt, stratification, solvent layer is separated, apply mechanically after dehydration, water layer filters, salts solution is through Multi-effect concentration, crystallization is filtered, apply mechanically after drying and crushing, filter cake drops in 2% hydrochloric acid soln, the quality of hydrochloric acid is 15 times of crude pigment product quality, at the temperature of 70 DEG C, 2h is boiled in acid, wash after filtration again, dry pigment finished product, diafiltration waste water directly enters wastewater treatment equipment and processes, rear discharge up to standard.
Described crude pigment product comprises phthalocyanine blue 15, pigment Violet 23, Pigment red 254, pigment blue 60, Pigment Yellow 73 110, pigment yellow 13 8.
Described inorganic salt are sodium-chlor.
Described organic solvent is water insoluble and grinds the organic solvent of inorganic salt solution used, the near saturated solution of density and grinding inorganic salt used not etc., can not produce obvious layering, optimum, machine solvent density is less than the near saturated solution grinding inorganic salt used, as toluene.
Embodiment 3
As shown in Figure 1, the method of a kind of efficient recovery grinding medium in pigmenting process of the present invention, comprise the steps: crude pigment product, inorganic salt, organic solvent adds in kneader or ball mill, crude pigment product, inorganic salt, the mass ratio of organic solvent is 1:8:1.5, 2h is ground at the temperature of 100 DEG C, abrasive is dropped in clear water and be heated to 50 DEG C of dissolvings, be configured to the saturated solution of inorganic salt, stratification, solvent layer is separated, apply mechanically after dehydration, water layer filters, salts solution is through Multi-effect concentration, crystallization is filtered, apply mechanically after drying and crushing, filter cake drops in 1% hydrochloric acid soln, the quality of hydrochloric acid is 30 times of crude pigment product quality, at the temperature of 100 DEG C, 1h is boiled in acid, wash after filtration again, dry pigment finished product, diafiltration waste water directly enters wastewater treatment equipment and processes, rear discharge up to standard.
Described crude pigment product comprises phthalocyanine green 15, pigment Violet 23, Pigment red 254, pigment blue 60, Pigment Yellow 73 110, pigment yellow 13 8.
Described inorganic salt are anhydrous sodium sulphate.
Described organic solvent is water insoluble and grinds the organic solvent of inorganic salt solution used, the near saturated solution of density and grinding inorganic salt used not etc., can not produce obvious layering, optimum, machine solvent density is less than the near saturated solution grinding inorganic salt used, as dimethylbenzene.
This technique is simple, and treatment effect is good, greatly can reduce the COD in factory effluent and saltiness, thus alleviate wastewater biochemical processing pressure.
Claims (7)
1. the method for an efficient recovery grinding medium in pigmenting process, it is characterized in that: comprise the steps: crude pigment product, inorganic salt, organic solvent adds in kneader or ball mill, 2-50h is ground at the temperature of 30-100 DEG C, abrasive is dropped in clear water and be heated to normal temperature-80 DEG C dissolving, be configured to the saturated solution of inorganic salt, stratification, solvent layer is separated, apply mechanically after dehydration, water layer filters, salts solution is through Multi-effect concentration, crystallization is filtered, apply mechanically after drying and crushing, filter cake drops in 1-3% hydrochloric acid soln, at the temperature of 50-100 DEG C, 1-3h is boiled in acid, wash after filtration again, dry pigment finished product, diafiltration waste water directly enters wastewater treatment equipment and processes, rear discharge up to standard,
Wherein, the mass ratio of described crude pigment product, inorganic salt, organic solvent is 1:(5-10): (1-2); The quality of described hydrochloric acid is 5-30 times of crude pigment product quality.
2. the method for a kind of efficient recovery grinding medium in pigmenting process according to claim 1, it is characterized in that: described crude pigment product comprises phthalocyanine pigment, dioxazine pigment, Isosorbide-5-Nitrae-diketopyrrolo-pyrrole pigment, condensed ring ketone pigment, isoindoline ketone pigment, quinophthalone class pigment.
3. the method for a kind of efficient recovery grinding medium in pigmenting process according to claim 2, it is characterized in that: described phthalocyanine pigment is phthalocyanine blue 15, described dioxazine pigment is pigment Violet 23, described 1,4-diketopyrrolo-pyrrole pigment is Pigment red 254, described condensed ring ketone pigment is pigment blue 60, and described isoindoline ketone pigment is Pigment Yellow 73 110, and described quinophthalone class pigment is pigment yellow 13 8.
4. the method for a kind of efficient recovery grinding medium in pigmenting process according to claim 1, is characterized in that: described inorganic salt are Calcium Chloride Powder Anhydrous, sodium-chlor or anhydrous sodium sulphate.
5. the method for a kind of efficient recovery grinding medium in pigmenting process according to claim 1, it is characterized in that: described organic solvent is water insoluble and grinds the organic solvent of inorganic salt solution used, the near saturated solution of density and grinding inorganic salt used not etc., can not produce obvious layering.
6. the method for a kind of efficient recovery grinding medium in pigmenting process according to claim 5, is characterized in that: described organic solvent density is less than the near saturated solution grinding inorganic salt used.
7. the method for a kind of efficient recovery grinding medium in pigmenting process according to claim 6, is characterized in that: described organic solvent is benzene, toluene or dimethylbenzene.
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| CN201310199817.1A CN103275517B (en) | 2013-05-27 | 2013-05-27 | Method for effectively recovering grinding medium in pigmentation process |
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| CN103275517B true CN103275517B (en) | 2015-06-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104629490A (en) * | 2014-12-31 | 2015-05-20 | 先尼科化工（上海）有限公司 | Environment-friendly grinding method of pigment salt |
| CN105111784B (en) * | 2015-09-28 | 2017-11-24 | 温州金源新材料科技有限公司 | The preparation method of high performance pigments indigo plant 60 |
| CN110835472A (en) * | 2018-08-18 | 2020-02-25 | 珠海东洋色材有限公司 | Manufacturing method for producing β type phthalocyanine blue pigment by high-energy ball milling equipment |
| CN110330045A (en) * | 2019-07-17 | 2019-10-15 | 曲靖众一合成化工有限公司 | A method of calcium chloride in recycling permanent violet refined wastewater |
| CN111548645B (en) * | 2020-03-02 | 2022-04-12 | 双乐颜料股份有限公司 | Activated phthalocyanine blue 15: 4 Process |
| CN115011138B (en) * | 2022-05-18 | 2023-11-17 | 宁夏彩妍科技有限公司 | Production method and production system of pigment red 177 for liquid crystal display screen |
| CN114958031A (en) * | 2022-06-30 | 2022-08-30 | 山东凯瑞尔光电科技有限公司 | Post-treatment method for yellow pigment kneading process of photoresist |
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| EP0072520A1 (en) * | 1981-08-14 | 1983-02-23 | Dainippon Ink And Chemicals, Inc. | Process for producing ground crude pigment |
| CN1310203A (en) * | 2001-02-20 | 2001-08-29 | 华东理工大学 | Synthesis of perylene pigment |
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| CN1916081A (en) * | 2006-08-25 | 2007-02-21 | 南通龙翔化工有限公司 | Production process of permanent violet RL |
| CN1958688A (en) * | 2006-11-24 | 2007-05-09 | 东华大学 | Nano pigment, preparation methd and application |
| WO2008116541A2 (en) * | 2007-03-23 | 2008-10-02 | Clariant Finance (Bvi) Limited | Method for producing transparent pigment violet 23 |
| CN102504567A (en) * | 2011-11-01 | 2012-06-20 | 东台市新锦泰化工有限公司 | Environment-friendly production method for permanent violet RL |
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2013
- 2013-05-27 CN CN201310199817.1A patent/CN103275517B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0072520A1 (en) * | 1981-08-14 | 1983-02-23 | Dainippon Ink And Chemicals, Inc. | Process for producing ground crude pigment |
| EP1411092A1 (en) * | 1999-07-09 | 2004-04-21 | Ciba Specialty Chemicals Holding Inc. | Highly crystalline pigment having an average particle size from 0.01 microm. to 0.12 microm. and improved colouristic properties |
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Address after: 226100 Nantong, Haimen City, Jiangsu Province, the new area of the Yangtze River Road, No. 88 Patentee after: Nantong Longxiang new materials Polytron Technologies Inc Address before: 226103 Jiangsu city of Nantong Province Haimen Development Zone, Haimen port Patentee before: Longxiang Chemical Co., Ltd., Nantong |
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Effective date of registration: 20220615 Address after: 226100 group 22, Tangxi village, Linjiang Town, Haimen District, Nantong City, Jiangsu Province Patentee after: Nantong longchen New Material Technology Co.,Ltd. Address before: 226100 No. 88, Yangzijiang Road, Linjiang new area, Haimen City, Nantong City, Jiangsu Province Patentee before: NANTONG LONGXIANG NEW MATERIALS TECHNOLOGY Co.,Ltd. |