CN112480709A - Production process of water-based velvet nigrosine - Google Patents
Production process of water-based velvet nigrosine Download PDFInfo
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- CN112480709A CN112480709A CN202011388080.4A CN202011388080A CN112480709A CN 112480709 A CN112480709 A CN 112480709A CN 202011388080 A CN202011388080 A CN 202011388080A CN 112480709 A CN112480709 A CN 112480709A
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- reaction
- nigrosine
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0097—Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B17/00—Azine dyes
- C09B17/02—Azine dyes of the benzene series
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a production process of aqueous velvet aniline black, which comprises the following steps: p1, adding aniline solid waste, an acidic compound and an oxidant into a reaction kettle, and carrying out an oxidation reaction to obtain a reaction mixture; p2, distilling the reaction mixture under reduced pressure to obtain a distilled mixture; p3, carrying out condensation reaction to obtain aniline black mixture with excessive aniline; p4, carrying out acidification reaction, and then carrying out centrifugal filtration to obtain nigrosine products and wastewater; p5, obtaining aniline black solution; p6, adding 25-35% by mass of PU resin into the nigrosine solution, uniformly stirring, and standing for 20-30 minutes to obtain a standing solution; p7, weighing 20-25% of fluff powder, putting into the standing solution, and stirring at a constant speed until the fluff powder is fully dispersed to obtain a mixed solution; p8, obtaining the velvet nigrosine, greatly improving the environmental protection effect by treating and recycling the wastewater, and being beneficial to production, popularization and use.
Description
Technical Field
The invention relates to the technical field of nigrosine, in particular to a production process of water-based velvet nigrosine.
Background
In the current industrial production, nigrosine, which is a chemical dye, has the characteristics of strong coloring, low dispersibility and good light absorption, and is widely applied to various fields for dyeing.
However, in the production and manufacturing process of nigrosine, the nigrosine is mostly prepared by directly mixing and reacting original raw materials, and in the existing raw material reaction structure, the proportion is unbalanced, so that the waste of the raw materials is caused by incomplete reaction, the raw materials cannot be recycled, meanwhile, the product cannot be subjected to post-treatment, the effect of nigrosine dyeing is reduced, and a new production process needs to be provided.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a production process of aqueous fluffy nigrosine.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production process of aqueous velvet aniline black comprises the following steps:
p1, adding aniline solid waste, an acidic compound and an oxidant into a reaction kettle, and carrying out an oxidation reaction to obtain a reaction mixture;
p2, distilling the reaction mixture under reduced pressure to obtain a distilled mixture;
p3, mixing the distilled mixture with nitrobenzene, and then carrying out condensation reaction in a condensation reaction kettle to obtain aniline black mixture with excessive aniline;
p4, putting the nigrosine mixture into an acidification reaction kettle, adding an acidic solution, carrying out acidification reaction, and then carrying out centrifugal filtration to obtain nigrosine products and wastewater;
p5, adding the nigrosine product into an isopropanol solvent, and uniformly stirring for 15 to 20 minutes to obtain a nigrosine solution;
p6, adding 25-35% by mass of PU resin into the nigrosine solution, uniformly stirring, and standing for 20-30 minutes to obtain a standing solution;
p7, weighing 20-25% of fluff powder, putting into the standing solution, and stirring at a constant speed until the fluff powder is fully dispersed to obtain a mixed solution;
and P8, heating the mixed solution to 120-130 ℃, distilling to remove the solvent, and then sieving and filtering to obtain the fluffy nigrosine.
Preferably, the mass percentage of the aniline solid waste, the acidic compound and the oxidant in the step P1 is 8-10:25-35: 3.
Preferably, the reduced pressure distillation pressure of the P2 step is-0.05 MPa to-0.08 MPa, and the distillation temperature is 50 ℃ to 75 ℃.
Preferably, the condensation reaction temperature of the step P3 is 150 to 180 ℃, and the reaction time is 3 to 5 hours.
Preferably, the acidification reaction in the step P4 adopts 8% hydrochloric acid solution, the reaction temperature is 120-140 ℃, and the reaction time is 120-150 minutes.
Preferably, the step P4 further comprises treating wastewater, comprising the steps of:
s1, inputting the wastewater into a treatment tower, and cooling by using circulating water at 15-20 ℃;
s2, standing the cooled wastewater for 2 to 3 hours, and carrying out layering treatment;
s3, separating the upper layer water for chemical purification;
s4, returning the lower aniline as the raw material to the P1 step for recycling as the raw material.
Preferably, the mass percentage content of the aniline in the lower layer in the step S4 is 85% -98%.
According to the production process of the water-based velvet nigrosine, the recycled solid waste raw materials are adopted for mixed reaction, and are controlled by combining various different reaction processes, so that the reaction efficiency is effectively improved, the raw materials which are not completely reacted can be recycled, the production cost is reduced, the velvet feeling treatment is performed on the product, the dyeing effect is improved, and meanwhile, the environment-friendly effect is greatly improved by treating and recycling the wastewater, so that the production process is beneficial to production, popularization and use.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A production process of aqueous velvet aniline black comprises the following steps:
p1, adding aniline solid waste, an acidic compound and an oxidant into a reaction kettle, and carrying out an oxidation reaction to obtain a reaction mixture;
p2, distilling the reaction mixture under reduced pressure to obtain a distilled mixture;
p3, mixing the distilled mixture with nitrobenzene, and then carrying out condensation reaction in a condensation reaction kettle to obtain aniline black mixture with excessive aniline;
p4, putting the nigrosine mixture into an acidification reaction kettle, adding an acidic solution, carrying out acidification reaction, and then carrying out centrifugal filtration to obtain nigrosine products and wastewater;
p5, adding the nigrosine product into an isopropanol solvent, and uniformly stirring for 15 to 20 minutes to obtain a nigrosine solution;
p6, adding 25-35% by mass of PU resin into the nigrosine solution, uniformly stirring, and standing for 20-30 minutes to obtain a standing solution;
p7, weighing 20-25% of fluff powder, putting into the standing solution, and stirring at a constant speed until the fluff powder is fully dispersed to obtain a mixed solution;
and P8, heating the mixed solution to 120-130 ℃, distilling to remove the solvent, and then sieving and filtering to obtain the fluffy nigrosine.
Preferably, the mass percentage of the aniline solid waste, the acidic compound and the oxidant in the step P1 is 8-10:25-35: 3.
Preferably, the reduced pressure distillation pressure of the P2 step is-0.05 MPa to-0.08 MPa, and the distillation temperature is 50 ℃ to 75 ℃.
Preferably, the condensation reaction temperature of the P3 step is 150 to 180 ℃, and the reaction time is 3 to 5 hours.
Preferably, the acidification reaction in the step P4 adopts 8% hydrochloric acid solution, the reaction temperature is 120-140 ℃, and the reaction time is 120-150 minutes.
Preferably, the step P4 further comprises treating the wastewater, comprising the steps of:
s1, inputting the wastewater into a treatment tower, and cooling by using circulating water at 15-20 ℃;
s2, standing the cooled wastewater for 2 to 3 hours, and carrying out layering treatment;
s3, separating the upper layer water for chemical purification;
s4, returning the lower aniline as the raw material to the P1 step for recycling as the raw material.
Preferably, the mass percentage content of the aniline in the lower layer in the step S4 is 85% -98%.
According to the production process of the water-based velvet nigrosine, the recycled solid waste raw materials are adopted for mixed reaction, and are controlled by combining various different reaction processes, so that the reaction efficiency is effectively improved, the raw materials which are not completely reacted can be recycled, the production cost is reduced, the velvet feeling treatment is performed on the product, the dyeing effect is improved, and meanwhile, the environment-friendly effect is greatly improved by treating and recycling the wastewater, so that the production process is beneficial to production, popularization and use.
Example 1
A production process of aqueous velvet aniline black comprises the following steps:
p1, adding aniline solid waste, an acidic compound and an oxidant into a reaction kettle, and carrying out an oxidation reaction to obtain a reaction mixture;
p2, distilling the reaction mixture under reduced pressure to obtain a distilled mixture;
p3, mixing the distilled mixture with nitrobenzene, and then carrying out condensation reaction in a condensation reaction kettle to obtain aniline black mixture with excessive aniline;
p4, putting the nigrosine mixture into an acidification reaction kettle, adding an acidic solution, carrying out acidification reaction, and then carrying out centrifugal filtration to obtain nigrosine products and wastewater;
p5, adding the nigrosine product into an isopropanol solvent, and uniformly stirring for 15 to 20 minutes to obtain a nigrosine solution;
p6, adding 30 mass percent of PU resin into the nigrosine solution, uniformly stirring, and standing for 20 to 30 minutes to obtain a standing solution;
p7, weighing 20% of fluff powder, putting into the standing solution, and stirring at a constant speed until the fluff powder is fully dispersed to obtain a mixed solution;
and P8, heating the mixed solution to 120-130 ℃, distilling to remove the solvent, and then sieving and filtering to obtain the fluffy nigrosine.
Preferably, the mass percentage of the aniline solid waste, the acidic compound and the oxidant in the step P1 is 9:35: 3.
Preferably, the reduced pressure distillation pressure of the P2 step is-0.05 MPa to-0.08 MPa, and the distillation temperature is 50 ℃ to 75 ℃.
Preferably, the condensation reaction temperature of the P3 step is 150 to 180 ℃, and the reaction time is 3 to 5 hours.
Preferably, the acidification reaction in the step P4 adopts 8% hydrochloric acid solution, the reaction temperature is 120-140 ℃, and the reaction time is 120-150 minutes.
Preferably, the step P4 further comprises treating the wastewater, comprising the steps of:
s1, inputting the wastewater into a treatment tower, and cooling by using circulating water at 15-20 ℃;
s2, standing the cooled wastewater for 2 to 3 hours, and carrying out layering treatment;
s3, separating the upper layer water for chemical purification;
s4, returning the lower aniline as the raw material to the P1 step for recycling as the raw material.
Preferably, the content of the aniline in the lower layer in the S4 step is 95% by mass.
Example 2
A production process of aqueous velvet aniline black comprises the following steps:
p1, adding aniline solid waste, an acidic compound and an oxidant into a reaction kettle, and carrying out an oxidation reaction to obtain a reaction mixture;
p2, distilling the reaction mixture under reduced pressure to obtain a distilled mixture;
p3, mixing the distilled mixture with nitrobenzene, and then carrying out condensation reaction in a condensation reaction kettle to obtain aniline black mixture with excessive aniline;
p4, putting the nigrosine mixture into an acidification reaction kettle, adding an acidic solution, carrying out acidification reaction, and then carrying out centrifugal filtration to obtain nigrosine products and wastewater;
p5, adding the nigrosine product into an isopropanol solvent, and uniformly stirring for 15 to 20 minutes to obtain a nigrosine solution;
p6, adding 28 mass percent of PU resin into the nigrosine solution, uniformly stirring, and standing for 20 to 30 minutes to obtain a standing solution;
p7, weighing 25% of fluff powder, putting into the standing solution, and stirring at a constant speed until the fluff powder is fully dispersed to obtain a mixed solution;
and P8, heating the mixed solution to 120-130 ℃, distilling to remove the solvent, and then sieving and filtering to obtain the fluffy nigrosine.
Preferably, the mass percentage of the aniline solid waste, the acidic compound and the oxidant in the step P1 is 8:30: 3.
Preferably, the reduced pressure distillation pressure of the P2 step is-0.05 MPa to-0.08 MPa, and the distillation temperature is 50 ℃ to 75 ℃.
Preferably, the condensation reaction temperature of the P3 step is 150 to 180 ℃, and the reaction time is 3 to 5 hours.
Preferably, the acidification reaction in the step P4 adopts 8% hydrochloric acid solution, the reaction temperature is 120-140 ℃, and the reaction time is 120-150 minutes.
Preferably, the step P4 further comprises treating the wastewater, comprising the steps of:
s1, inputting the wastewater into a treatment tower, and cooling by using circulating water at 15-20 ℃;
s2, standing the cooled wastewater for 2 to 3 hours, and carrying out layering treatment;
s3, separating the upper layer water for chemical purification;
s4, returning the lower aniline as the raw material to the P1 step for recycling as the raw material.
Preferably, the content of the aniline in the lower layer in the step S4 is 88% by mass.
Claims (7)
1. A production process of water-based velvet aniline black is characterized by comprising the following steps: the production process comprises the following steps:
p1, adding aniline solid waste, an acidic compound and an oxidant into a reaction kettle, and carrying out an oxidation reaction to obtain a reaction mixture;
p2, distilling the reaction mixture under reduced pressure to obtain a distilled mixture;
p3, mixing the distilled mixture with nitrobenzene, and then carrying out condensation reaction in a condensation reaction kettle to obtain aniline black mixture with excessive aniline;
p4, putting the nigrosine mixture into an acidification reaction kettle, adding an acidic solution, carrying out acidification reaction, and then carrying out centrifugal filtration to obtain nigrosine products and wastewater;
p5, adding the nigrosine product into an isopropanol solvent, and uniformly stirring for 15 to 20 minutes to obtain a nigrosine solution;
p6, adding 25-35% by mass of PU resin into the nigrosine solution, uniformly stirring, and standing for 20-30 minutes to obtain a standing solution;
p7, weighing 20-25% of fluff powder, putting into the standing solution, and stirring at a constant speed until the fluff powder is fully dispersed to obtain a mixed solution;
and P8, heating the mixed solution to 120-130 ℃, distilling to remove the solvent, and then sieving and filtering to obtain the fluffy nigrosine.
2. The production process of the aqueous velvet aniline black according to the claim 1, which is characterized in that: the mass percentage of the aniline solid waste, the acidic compound and the oxidant in the step P1 is 8-10:25-35: 3.
3. The production process of the aqueous velvet aniline black according to the claim 1, which is characterized in that: and the reduced pressure distillation pressure of the step P2 is-0.05 MPa to-0.08 MPa, and the distillation temperature is 50 ℃ to 75 ℃.
4. The production process of the aqueous velvet aniline black according to the claim 1, which is characterized in that: the condensation reaction temperature of the step P3 is 150-180 ℃, and the reaction time is 3-5 hours.
5. The production process of the aqueous velvet aniline black according to the claim 1, which is characterized in that: the acidification reaction in the step P4 adopts hydrochloric acid solution with the concentration of 8%, the reaction temperature is 120-140 ℃, and the reaction time is 120-150 minutes.
6. The production process of the aqueous velvet aniline black according to the claim 1, which is characterized in that: the P4 step further comprises the step of treating the wastewater, comprising the following steps:
s1, inputting the wastewater into a treatment tower, and cooling by using circulating water at 15-20 ℃;
s2, standing the cooled wastewater for 2 to 3 hours, and carrying out layering treatment;
s3, separating the upper layer water for chemical purification;
s4, returning the lower aniline as the raw material to the P1 step for recycling as the raw material.
7. The production process of the aqueous velvet aniline black according to claim 6, characterized in that: the mass percentage content of the lower aniline in the step S4 is 85% -98%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011388080.4A CN112480709A (en) | 2020-12-02 | 2020-12-02 | Production process of water-based velvet nigrosine |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011388080.4A CN112480709A (en) | 2020-12-02 | 2020-12-02 | Production process of water-based velvet nigrosine |
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| CN112480709A true CN112480709A (en) | 2021-03-12 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3000529A1 (en) * | 1980-01-09 | 1981-07-16 | Bayer Ag, 5090 Leverkusen | METHOD FOR PRODUCING ANILINE CONDENSATION DYES |
| CN103015186A (en) * | 2012-12-24 | 2013-04-03 | 建德市顺发化工助剂有限公司 | Carbon black treating agent for synthetic leather and preparation method of carbon black treating agent |
| CN103896864A (en) * | 2014-04-23 | 2014-07-02 | 青岛双桃精细化工（集团）有限公司 | Preparation method of nigrosine |
| CN104131466A (en) * | 2014-07-22 | 2014-11-05 | 嘉兴禾大科技化学有限公司 | Velvet feeling polyurethane leather surface conditioning agent and preparation method thereof |
| CN104610173A (en) * | 2015-01-13 | 2015-05-13 | 青岛双桃精细化工（集团）有限公司 | Recycling production process for nigrosine |
-
2020
- 2020-12-02 CN CN202011388080.4A patent/CN112480709A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3000529A1 (en) * | 1980-01-09 | 1981-07-16 | Bayer Ag, 5090 Leverkusen | METHOD FOR PRODUCING ANILINE CONDENSATION DYES |
| CN103015186A (en) * | 2012-12-24 | 2013-04-03 | 建德市顺发化工助剂有限公司 | Carbon black treating agent for synthetic leather and preparation method of carbon black treating agent |
| CN103896864A (en) * | 2014-04-23 | 2014-07-02 | 青岛双桃精细化工（集团）有限公司 | Preparation method of nigrosine |
| CN104131466A (en) * | 2014-07-22 | 2014-11-05 | 嘉兴禾大科技化学有限公司 | Velvet feeling polyurethane leather surface conditioning agent and preparation method thereof |
| CN104610173A (en) * | 2015-01-13 | 2015-05-13 | 青岛双桃精细化工（集团）有限公司 | Recycling production process for nigrosine |
Non-Patent Citations (1)
| Title |
|---|
| 王锡娇: "《涂料与颜料标准应用手册》", 30 April 2005 * |
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Address after: 323000 No.2 Huimin street, Shuige Industrial Zone, Liandu District, Lishui City, Zhejiang Province Applicant after: Zhejiang Zhongda New Material Co.,Ltd. Address before: 323000 No.2 Huimin street, Shuige Industrial Zone, Liandu District, Lishui City, Zhejiang Province Applicant before: Lishui Dacheng New Material Co.,Ltd. |
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Application publication date: 20210312 |