CN115011140A - High-yield vulcanized black processing technology - Google Patents
High-yield vulcanized black processing technology Download PDFInfo
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- CN115011140A CN115011140A CN202210751000.XA CN202210751000A CN115011140A CN 115011140 A CN115011140 A CN 115011140A CN 202210751000 A CN202210751000 A CN 202210751000A CN 115011140 A CN115011140 A CN 115011140A
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- black
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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
- C09B49/00—Sulfur dyes
- C09B49/06—Sulfur dyes from azines, oxazines, thiazines or thiazoles
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention relates to the technical field of processing of sulfur black, and discloses a high-yield processing technology of sulfur black, which comprises the following steps: carrying out hydrolysis reaction on 2, 4-dinitrochlorobenzene and liquid caustic soda in a hydrolysis kettle to generate 2, 4-dinitrophenol sodium, sodium chloride and water; adding the hydrolysate and the prepared sodium polysulfide into a vulcanizing kettle for vulcanization reaction; then pressing the vulcanized liquid into an oxidation kettle, introducing air into the oxidation kettle for oxidation reaction, and then performing filter pressing, size mixing and drying to obtain a product, namely vulcanized black; the processing technology of the vulcanized black with high yield can achieve the effect of recycling the waste water, reduce the usage amount of liquid caustic soda (sodium hydroxide) in the hydrolysis technology of the vulcanized black, improve the yield, add the mother liquor for producing the 2-amino-4-nitrophenol sodium into a vulcanizing kettle, use the mother liquor to make the vulcanized black of the produced finished product better, and save the usage amount of the vulcanized alkali and the sulfur.
Description
Technical Field
The invention relates to the technical field of vulcanized black, in particular to a high-yield vulcanized black processing technology.
Background
Sulfur black, also known as sulfur cyan, is a black dye. The sulfur black is prepared by hydrolyzing 2, 4-dinitrochlorobenzene with a sodium hydroxide solution to generate 2, 4-dinitrophenol sodium and then carrying out a vulcanization reaction with sodium sulfide. The sulfur black dye is a high molecular compound containing more sulfur, the structure of the sulfur black dye contains disulfide bonds and polysulfide bonds, and the sulfur black dye is unstable, particularly, the polysulfide bonds can be oxidized into sulfur oxides by oxygen in the air under certain temperature and humidity conditions, and further react with water molecules in the air to generate sulfuric acid, so that the strength of the yarn is reduced, the fiber is brittle, and the fiber is completely embrittled into powder in serious cases, so that the yarn dyed by the sulfur black dye is used for reducing or preventing the brittle of the fiber;
the traditional processing technology of the sulfur black can not achieve the effect of recycling the waste water generated in the production, and the produced hydrolysis technology of the sulfur black has more usage amount of liquid caustic soda (sodium hydroxide) and lower yield;
therefore, a high-yield processing technology of the vulcanized black is urgently needed to solve the above-mentioned defects.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high-yield vulcanized black processing technology, and solves the problems that the traditional vulcanized black processing technology cannot achieve the effect of recycling, and the produced vulcanized black hydrolysis technology has more usage amount of liquid caustic soda (sodium hydroxide) and lower yield.
The invention provides the following technical scheme: a processing technology of sulfur black with high yield comprises the following steps:
step one, performing hydrolysis reaction on 2, 4-dinitrochlorobenzene and liquid caustic soda in a hydrolysis kettle to generate 2, 4-dinitrophenol sodium, sodium chloride and water;
secondly, adding the hydrolysate and the prepared sodium polysulfide into a vulcanizing kettle for vulcanization reaction;
and step three, pressing the sulfide liquid into an oxidation kettle, introducing air into the oxidation kettle to perform oxidation reaction, and performing filter pressing, size mixing and drying to obtain the product sulfide black.
Preferably, the process wastewater from the 2, 4-dinitrochlorobenzene production is used as the bottom water of the hydrolysis process in the process for producing the vulcanized black, and each batch has a volume of 7.5m 3 And the content of sodium carbonate in the process wastewater is below 1.8 percent.
Preferably, the mother liquor for producing the 2-amino-4-sodium nitrophenolate is added into a vulcanizing kettle for use, and each batch is 5m 3 。
Preferably, the hydrolysis reaction in step one is of the formula
Preferably, the chemical reaction equation for the preparation of sodium polysulfide is Na 2 S+(X-1)
S＝Na 2 Sx-268kJ/kmol。
Preferably, the production of the sulfur black comprises the following chemical reaction equation:
compared with the prior art, the invention has the following beneficial effects:
the invention has the advantages that: the process waste water can achieve the effect of recycling, reduce the usage amount of liquid caustic soda (sodium hydroxide) in the hydrolysis process of producing the vulcanized black, and simultaneously can improve the yield, the mother liquor for producing the 2-amino-4-nitrophenol sodium is added into a vulcanizing kettle, the treatment of the mother liquor for producing the 2-amino-4-nitrophenol sodium is omitted, the produced finished product has better vulcanized black light by using the mother liquor, and the usage amount of the sodium sulfide and the sulfur is saved.
Drawings
Other features, objects and advantages of the present application will become more apparent upon reading of the following detailed description of non-limiting embodiments thereof, made with reference to the accompanying drawings in which:
FIG. 1 is a flow chart of a high yield process for producing sulfur black according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The drawings are only for purposes of illustration and are not intended to be limiting, certain elements of the drawings may be omitted, enlarged or reduced to better illustrate the embodiments of the present invention, and do not represent the size of the actual product, and it is understood that some well-known structures, elements and descriptions thereof in the drawings may be omitted for persons skilled in the art.
In the description of the present invention, it should be further noted that, unless otherwise explicitly stated or limited, the terms "disposed" and "connected" should be interpreted broadly, and may be, for example, a fixed connection, a movable connection, a detachable connection, an integrated connection, a mechanical connection, an electrical connection, a direct connection, an indirect connection via an intermediate medium, and a communication between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
Referring to fig. 1, a process for producing high yield sulfur black includes the following steps:
step one, performing hydrolysis reaction on 2, 4-dinitrochlorobenzene and liquid caustic soda in a hydrolysis kettle to generate 2, 4-dinitrophenol sodium, sodium chloride and water;
secondly, adding the hydrolysate and the prepared sodium polysulfide into a vulcanizing kettle for vulcanization reaction;
and step three, pressing the sulfide liquid into an oxidation kettle, introducing air into the oxidation kettle to perform oxidation reaction, and performing filter pressing, size mixing and drying to obtain the product sulfide black.
Wherein, the process wastewater from the production of 2, 4-dinitrochlorobenzene is used as the bottom water of the hydrolysis process in the production of the vulcanized black, and each batch has a volume of 7.5m 3 The content of sodium carbonate in the process wastewater is required to be below 1.8 percent, the hydrolysis reaction utilizes the process wastewater of the 2, 4-dinitrochlorobenzene to recover the 2, 4-dinitrochlorobenzene which is slightly dissolved in the process wastewater and the alkali in the wastewater, and the usage amount of the 2, 4-dinitrochlorobenzene and liquid alkali is reduced.
Wherein, mother liquor for producing 2-amino-4-sodium nitrophenolate is added into a vulcanizing kettle for use, and each batch is 5m 3 . Mother liquor for producing 2-amino-4-nitrophenol sodium is added into a polysulfide kettle, the yield of polysulfide can be improved by utilizing the 2, 4-dinitrophenol sodium which does not react completely in the production of the 2-amino-4-nitrophenol sodium, and the consumption of sodium sulfide can be reduced by utilizing the excessive sodium hydrosulfide in the mother liquor of the 2-amino-4-nitrophenol sodium.
Wherein the hydrolysis reaction equation in the first step is
Wherein the chemical reaction equation for preparing sodium polysulfide is Na 2 S+(X-1)
S＝Na 2 Sx-268kJ/kmol。
Wherein, the production of the sulfur black comprises the following chemical reaction equation:
it should be noted that, the waste water from the process can not only achieve the effect of recycling, reduce the usage amount of liquid caustic soda (sodium hydroxide) in the hydrolysis process of producing vulcanized black, but also improve the yield, and the mother liquor for producing 2-amino-4-nitrophenol sodium is used as the bottom water of the vulcanization process, and the mother liquor is used as the bottom water to make the vulcanized black light of the finished product better, and save the usage amount of the sodium sulfide and sulfur, and the content not described in detail in the description belongs to the prior art known by the professional technicians in the field.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The processing technology of the sulfur black with high yield is characterized by comprising the following steps:
step one, performing hydrolysis reaction on 2, 4-dinitrochlorobenzene and liquid caustic soda in a hydrolysis kettle to generate 2, 4-dinitrophenol sodium, sodium chloride and water;
secondly, adding the hydrolysate and the prepared sodium polysulfide into a vulcanizing kettle for vulcanization reaction;
and step three, pressing the sulfide liquid into an oxidation kettle, introducing air into the oxidation kettle to perform oxidation reaction, and performing filter pressing, size mixing and drying to obtain the product sulfide black.
2. The process of claim 1, wherein the step of processing the vulcanized black comprises: the process wastewater from the production of 2, 4-dinitrochlorobenzene is used as the bottom water of the hydrolysis process in the production of the vulcanized black, and each batch has a volume of 7.5m 3 The content of soda ash (sodium carbonate) in the process wastewater is required to be below 1.8%.
3. The process of claim 1, wherein the step of processing the vulcanized black comprises: the mother liquor for producing the 2-amino-4-sodium nitrophenolate is added into a vulcanizing kettle for use, and each batch is 5m 3 。
4. The process of claim 1, wherein the step of processing the vulcanized black comprises: the hydrolysis reaction equation in the first step is
5. The process of claim 1, wherein the step of processing the vulcanized black comprises the following steps: the chemical reaction equation for the preparation of sodium polysulfide is Na 2 S+(X-1)S＝Na 2 Sx-268kJ/kmol。
6. The process of claim 1, wherein the step of processing the vulcanized black comprises: the production of the sulfur black comprises the following chemical reaction equation:
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| CN202210751000.XA CN115011140A (en) | 2022-06-28 | 2022-06-28 | High-yield vulcanized black processing technology |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB364048A (en) * | 1930-09-24 | 1931-12-24 | Du Pont | Improvements in or relating to the manufacture of sulphide blacks |
| EP0741168A1 (en) * | 1995-05-03 | 1996-11-06 | Clariant Finance (BVI) Limited | Sulphur dyes |
| CN1513830A (en) * | 2003-07-29 | 2004-07-21 | 徐德军 | Preparation method of 2,4-dinitochloro benzene |
| CN1786079A (en) * | 2004-12-27 | 2006-06-14 | 阮加根 | Preparation process of sulfur black dye and product thereof |
| CN102516796A (en) * | 2011-11-21 | 2012-06-27 | 苏州贵族公子服饰有限公司 | Preparation method for vulcanized reactive dye |
| CN111100475A (en) * | 2020-01-08 | 2020-05-05 | 山西临汾染化(集团)有限责任公司 | Preparation method of sulfur dye |
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2022
- 2022-06-28 CN CN202210751000.XA patent/CN115011140A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB364048A (en) * | 1930-09-24 | 1931-12-24 | Du Pont | Improvements in or relating to the manufacture of sulphide blacks |
| EP0741168A1 (en) * | 1995-05-03 | 1996-11-06 | Clariant Finance (BVI) Limited | Sulphur dyes |
| CN1513830A (en) * | 2003-07-29 | 2004-07-21 | 徐德军 | Preparation method of 2,4-dinitochloro benzene |
| CN1786079A (en) * | 2004-12-27 | 2006-06-14 | 阮加根 | Preparation process of sulfur black dye and product thereof |
| CN102516796A (en) * | 2011-11-21 | 2012-06-27 | 苏州贵族公子服饰有限公司 | Preparation method for vulcanized reactive dye |
| CN111100475A (en) * | 2020-01-08 | 2020-05-05 | 山西临汾染化(集团)有限责任公司 | Preparation method of sulfur dye |
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