CN103275517A - 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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- CN103275517A CN103275517A CN2013101998171A CN201310199817A CN103275517A CN 103275517 A CN103275517 A CN 103275517A CN 2013101998171 A CN2013101998171 A CN 2013101998171A CN 201310199817 A CN201310199817 A CN 201310199817A CN 103275517 A CN103275517 A CN 103275517A
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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, relate in particular to a kind of in the pigmenting process method of efficient recovery grinding medium.
Background technology
Pigment dyestuff generally is distributed in the coloring medium with the minuteness particle form, physical factors such as the crystal formation of pigment particles, shape, size and condition of surface all can influence reflection of light, absorption and scattering, thereby influence coloured light, tinting strength, opacifying power and dispersiveness, also can its performances such as fast light, heat-resisting, weather be impacted simultaneously.
Crude pigment product crystal stability by chemosynthesis is poor, add that the crude product particle is big, thereby tinting strength is low, should not be used as commodity pigment, must carry out pigmenting (commercialization) and handle, reduce its globule size, and make it be converted into stable performance, strong coloring force, the stable state crystal that coloured light is bright-coloured.
Pigmenting generally divides sour dissolved method and polishing.Acid dissolved method (US4317908, US4804417) is with the crude pigment product dissolving or is partially dissolved in the vitriol oil, pour into then in the big water gaging, it is separated out with fine crystals, be translated into stable crystal formation through solvent treatment again, improve crystal surface morphology simultaneously, can obtain the pigment finished product of excellent performance.Produce the sulfuric acid of big volume low-concentration in the acid dissolved method process, therefore wastewater treatment difficulty, cost height seldom adopt.Polishing (US6517630B1, US20100101456A1) grinds crude pigment product with inorganic salt and organic solvent, boil by acid, can directly obtain the pigment finished product of excellent performance.Polishing need add a large amount of inorganic salt (5-10 is doubly to crude pigment product usually) grinding aid and organic solvent (1-2 is doubly to crude pigment product), and brine waste easily causes microorganism wall to break, thereby has a strong impact on the wastewater biochemical treatment effect.
Summary of the invention
The purpose of this invention is to provide a kind of in the pigmenting process method of efficient recovery grinding medium.
The technical solution used in the present invention is:
A kind of in the pigmenting process method of efficient recovery grinding medium, comprise the steps: crude pigment product, inorganic salt, organic solvent adds in kneader or the ball mill, under 30-100 ℃ temperature, grind 2-50h, abrasive dropped into be heated to normal temperature-80 ℃ dissolving in the clear water, be configured to the saturated solution of inorganic salt, standing demix, solvent layer is told, after dehydration, apply mechanically, water layer filters, salts solution concentrates through multiple-effect, crystallization is filtered, apply mechanically after the drying and crushing, filter cake drops in the 1-3% hydrochloric acid soln, and 1-3h is boiled in acid under 50-100 ℃ temperature, again washing after filtration, the dry pigment finished product that gets, diafiltration waste water directly enters wastewater treatment equipment and handles, back up to standard discharging.
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, 1,4-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, the 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 used inorganic salt solution that density does not wait with the near saturated solution that grinds used inorganic salt, can produce obvious layering.
Described organic solvent density is less than the near saturated solution that grinds used inorganic salt.
Described organic solvent is benzene, toluene or dimethylbenzene.
Advantage of the present invention is: this technology is simple, and treatment effect is good, can reduce COD and saltiness in the factory effluent greatly, thereby alleviates the wastewater biochemical processing pressure.
Description of drawings
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, of the present invention a kind of in the pigmenting process method of efficient recovery grinding medium, comprise the steps: crude pigment product, inorganic salt, organic solvent adds in kneader or the ball mill, crude pigment product, inorganic salt, the mass ratio of organic solvent is 1:5:1, under 30 ℃ temperature, grind 40h, abrasive dropped into be heated to 70 ℃ of dissolvings in the clear water, be configured to the saturated solution of inorganic salt, standing demix is told solvent layer, applies mechanically after dehydration, water layer filters, salts solution concentrates through multiple-effect, crystallization is filtered, apply mechanically after the drying and crushing, filter cake drops in 3% hydrochloric acid soln, and the quality of hydrochloric acid is 5 times of crude pigment product quality, 3h is boiled in acid under 50 ℃ temperature, washing after filtration again, the dry pigment finished product that gets, diafiltration waste water directly enters wastewater treatment equipment and handles, back up to standard discharging.。
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 used inorganic salt solution, density does not wait with the near saturated solution that grinds used inorganic salt, can produce obvious layering, optimum, the machine solvent density is less than the near saturated solution that grinds used inorganic salt, as benzene.
Embodiment 2
As shown in Figure 1, of the present invention a kind of in the pigmenting process method of efficient recovery grinding medium, comprise the steps: crude pigment product, inorganic salt, organic solvent adds in kneader or the ball mill, crude pigment product, inorganic salt, the mass ratio of organic solvent is 1:10:2, under 50 ℃ temperature, grind 20h, abrasive dropped into be heated to 30 ℃ of dissolvings in the clear water, be configured to the saturated solution of inorganic salt, standing demix is told solvent layer, applies mechanically after dehydration, water layer filters, salts solution concentrates through multiple-effect, crystallization is filtered, apply mechanically after the drying and crushing, filter cake drops in 2% hydrochloric acid soln, and the quality of hydrochloric acid is 15 times of crude pigment product quality, 2h is boiled in acid under 70 ℃ temperature, washing after filtration again, the dry pigment finished product that gets, diafiltration waste water directly enters wastewater treatment equipment and handles, back up to standard discharging.
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 used inorganic salt solution, density does not wait with the near saturated solution that grinds used inorganic salt, can produce obvious layering, optimum, the machine solvent density is less than the near saturated solution that grinds used inorganic salt, as toluene.
Embodiment 3
As shown in Figure 1, of the present invention a kind of in the pigmenting process method of efficient recovery grinding medium, comprise the steps: crude pigment product, inorganic salt, organic solvent adds in kneader or the ball mill, crude pigment product, inorganic salt, the mass ratio of organic solvent is 1:8:1.5, under 100 ℃ temperature, grind 2h, abrasive dropped into be heated to 50 ℃ of dissolvings in the clear water, be configured to the saturated solution of inorganic salt, standing demix is told solvent layer, applies mechanically after dehydration, water layer filters, salts solution concentrates through multiple-effect, crystallization is filtered, apply mechanically after the drying and crushing, filter cake drops in 1% hydrochloric acid soln, and the quality of hydrochloric acid is 30 times of crude pigment product quality, 1h is boiled in acid under 100 ℃ temperature, washing after filtration again, the dry pigment finished product that gets, diafiltration waste water directly enters wastewater treatment equipment and handles, back up to standard discharging.
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 used inorganic salt solution, density does not wait with the near saturated solution that grinds used inorganic salt, can produce obvious layering, optimum, the machine solvent density is less than the near saturated solution that grinds used inorganic salt, as dimethylbenzene.
This technology is simple, and treatment effect is good, can reduce COD and saltiness in the factory effluent greatly, thereby alleviates the wastewater biochemical processing pressure.
Claims (9)
1. the method for an efficient recovery grinding medium in the pigmenting process, it is characterized in that: comprise the steps: crude pigment product, inorganic salt, organic solvent adds in kneader or the ball mill, under 30-100 ℃ temperature, grind 2-50h, abrasive dropped into be heated to normal temperature-80 ℃ dissolving in the clear water, be configured to the saturated solution of inorganic salt, standing demix, solvent layer is told, after dehydration, apply mechanically, water layer filters, salts solution concentrates through multiple-effect, crystallization is filtered, apply mechanically after the drying and crushing, filter cake drops in the 1-3% hydrochloric acid soln, and 1-3h is boiled in acid under 50-100 ℃ temperature, again washing after filtration, the dry pigment finished product that gets, diafiltration waste water directly enters wastewater treatment equipment and handles, back up to standard discharging.
According to claim 1 a kind of in the pigmenting process method of efficient recovery grinding medium, it is characterized in that: the mass ratio of described crude pigment product, inorganic salt, organic solvent is 1:(5-10): (1-2).
According to claim 1 a kind of in the pigmenting process method of efficient recovery grinding medium, it is characterized in that: the quality of described hydrochloric acid be the crude pigment product quality 5-30 doubly.
According to claim 1 a kind of in the pigmenting process method of efficient recovery grinding medium, it is characterized in that: described crude pigment product comprises phthalocyanine pigment, dioxazine pigment, 1,4-diketopyrrolo-pyrrole pigment, condensed ring ketone pigment, isoindoline ketone pigment, quinophthalone class pigment.
According to claim 4 a kind of in the pigmenting process method of efficient recovery grinding medium, it is characterized in that: described phthalocyanine pigment is phthalocyanine blue 15, described dioxazine pigment is pigment Violet 23, described 1, the 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.
According to claim 1 a kind of in the pigmenting process method of efficient recovery grinding medium, it is characterized in that: described inorganic salt are Calcium Chloride Powder Anhydrous, sodium-chlor or anhydrous sodium sulphate.
According to claim 1 a kind of in the pigmenting process method of efficient recovery grinding medium, it is characterized in that: described organic solvent is water insoluble and grinds the organic solvent of used inorganic salt solution, density does not wait with the near saturated solution that grinds used inorganic salt, can produce obvious layering.
According to claim 7 a kind of in the pigmenting process method of efficient recovery grinding medium, it is characterized in that: described organic solvent density is less than the near saturated solution that grinds used inorganic salt.
According to claim 8 a kind of in the pigmenting process method of efficient recovery grinding medium, it is characterized in that: described organic solvent is benzene, toluene or dimethylbenzene.
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Cited By (7)
| 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 |
| CN105111784A (en) * | 2015-09-28 | 2015-12-02 | 温州金源化工有限公司 | Preparation method of high-performance pigment blue 60 |
| 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 |
| 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 |
| CN111548645A (en) * | 2020-03-02 | 2020-08-18 | 双乐颜料股份有限公司 | Activated phthalocyanine blue 15: 4 Process |
| 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 |
| CN115011138A (en) * | 2022-05-18 | 2022-09-06 | 宁夏彩妍科技有限公司 | Production method and production system of pigment red 177 for liquid crystal display screen |
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| EP0072520A1 (en) * | 1981-08-14 | 1983-02-23 | Dainippon Ink And Chemicals, Inc. | Process for producing ground crude pigment |
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Cited By (10)
| 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 |
| CN105111784A (en) * | 2015-09-28 | 2015-12-02 | 温州金源化工有限公司 | Preparation method of high-performance pigment blue 60 |
| 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 |
| CN111548645A (en) * | 2020-03-02 | 2020-08-18 | 双乐颜料股份有限公司 | Activated phthalocyanine blue 15: 4 Process |
| CN111548645B (en) * | 2020-03-02 | 2022-04-12 | 双乐颜料股份有限公司 | Activated phthalocyanine blue 15: 4 Process |
| CN115011138A (en) * | 2022-05-18 | 2022-09-06 | 宁夏彩妍科技有限公司 | Production method and production system of pigment red 177 for liquid crystal display screen |
| 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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| CN103275517B (en) | 2015-06-03 |
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