WO2022236795A1 - 一种染料分散蓝b56#的生产方法 - Google Patents
一种染料分散蓝b56#的生产方法 Download PDFInfo
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- WO2022236795A1 WO2022236795A1 PCT/CN2021/093755 CN2021093755W WO2022236795A1 WO 2022236795 A1 WO2022236795 A1 WO 2022236795A1 CN 2021093755 W CN2021093755 W CN 2021093755W WO 2022236795 A1 WO2022236795 A1 WO 2022236795A1
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- Prior art keywords
- disperse blue
- hydrolysis
- production method
- dinitrophenol
- mother liquor
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 35
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 44
- 230000007062 hydrolysis Effects 0.000 claims abstract description 42
- 239000012452 mother liquor Substances 0.000 claims abstract description 35
- 239000012065 filter cake Substances 0.000 claims abstract description 32
- 239000000975 dye Substances 0.000 claims abstract description 27
- UFBJCMHMOXMLKC-UHFFFAOYSA-N 2,4-dinitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O UFBJCMHMOXMLKC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000006227 byproduct Substances 0.000 claims abstract description 16
- 239000000047 product Substances 0.000 claims abstract description 16
- 238000007670 refining Methods 0.000 claims abstract description 16
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 230000031709 bromination Effects 0.000 claims abstract description 7
- 238000005893 bromination reaction Methods 0.000 claims abstract description 7
- 238000009833 condensation Methods 0.000 claims abstract description 7
- 230000005494 condensation Effects 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 230000009467 reduction Effects 0.000 claims abstract description 7
- 238000012958 reprocessing Methods 0.000 claims abstract description 7
- 235000010265 sodium sulphite Nutrition 0.000 claims abstract description 7
- 230000009466 transformation Effects 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 36
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 32
- 239000002253 acid Substances 0.000 claims description 14
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 2
- 229910017604 nitric acid Inorganic materials 0.000 claims 2
- 238000001514 detection method Methods 0.000 claims 1
- 238000000746 purification Methods 0.000 claims 1
- 238000006722 reduction reaction Methods 0.000 claims 1
- 229910002651 NO3 Inorganic materials 0.000 abstract description 12
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract description 12
- 238000011084 recovery Methods 0.000 abstract description 6
- 239000002699 waste material Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 5
- JMOHQJVXBQAVNW-UHFFFAOYSA-M sodium;2,4-dinitrophenolate Chemical compound [Na+].[O-]C1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O JMOHQJVXBQAVNW-UHFFFAOYSA-M 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 239000000543 intermediate Substances 0.000 abstract description 3
- 230000020477 pH reduction Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 239000002920 hazardous waste Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- KHUFHLFHOQVFGB-UHFFFAOYSA-N 1-aminoanthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2N KHUFHLFHOQVFGB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/16—Separation; Purification; Stabilisation; Use of additives
-
- 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
- C09B1/00—Dyes with anthracene nucleus not condensed with any other ring
- C09B1/50—Amino-hydroxy-anthraquinones; Ethers and esters thereof
- C09B1/503—Amino-hydroxy-anthraquinones; Ethers and esters thereof unsubstituted amino-hydroxy anthraquinone
Definitions
- the invention belongs to the technical field of chemical dyes, and in particular relates to a production method of dye disperse blue B56#.
- the technical problem to be solved in the present invention is to provide a kind of production method of dye disperse blue B56#, effectively utilize the active ingredient in the mother liquor of hydrolysis recovery, reduce three waste discharges, produce by-product by acidification, filtration 2-4-Dinitrophenol.
- a kind of production method of dye disperse blue B56# by utilizing sodium sulfite to treat 1-aminoanthraquinone DMF residue to purify and produce mixed nitrate, then the mixed nitrate is sequentially passed through mononitration, mononitration refining, condensation, dinitration, hydrolysis, reduction and In the process of bromination transformation, the product disperse blue B56# is finally obtained; the mother liquor recovered by hydrolysis is reprocessed to recover the by-product 2,4-dinitrophenol.
- the production method of the dye disperse blue B56#, the reprocessing of the reclaimed mother liquor by hydrolysis specifically comprises the following steps:
- step (2) Add activated carbon to the solution in step (1), stir and decolorize for 0.5 to 1 hour;
- the production method of the dye disperse blue B56# the step (1) adding sulfuric acid to adjust the solution to a pH value of 4-7.
- the filtrate in the step (3) is added to an acid adjustment tank to adjust the pH to ⁇ 1.0.
- the reaction temperature in the step (1) is 60-70° C., and the reaction time is 0.5-1 h.
- the mass fraction of the sulfuric acid is 90% to 98%, and the amount of the sulfuric acid is 40% to 50% of the mass of the mother liquor recovered by hydrolysis.
- the ratio of the amount of activated carbon used in the step (2) to the mass of the recovered mother liquor by hydrolysis is 1:3 to 1:5.
- the advantages of the present invention include:
- Disperse blue B56# filter cake hydrolysis reaction process of the present invention produces 2,4-dinitrophenol sodium salt, and 2,4-dinitrophenol sodium salt is dissolved in the mother liquor recovered by hydrolysis, in order to effectively utilize the active ingredients therein, Reduce the discharge of three wastes, and produce the by-product 2-4-dinitrophenol through acidification and filtration.
- the by-products all meet the standards and can be used as raw materials for the production of coating intermediates.
- a kind of production method of dye disperse blue B56# by utilizing sodium sulfite to treat 1-aminoanthraquinone DMF residue to purify and produce mixed nitrate, then the mixed nitrate is sequentially passed through mononitration, mononitration refining, condensation, dinitration, hydrolysis, reduction and In the process of bromination transformation, the product disperse blue B56# is finally obtained; the mother liquor recovered by hydrolysis is reprocessed to recover the by-product 2,4-dinitrophenol.
- the reprocessing of the recovered mother liquor by hydrolysis specifically includes the following steps:
- step (2) Add activated carbon to the solution of step (1), stir and decolorize for 0.8h; the ratio of the consumption of activated carbon to the quality of the hydrolysis recovery mother liquor is 1:3;
- the material is pumped into an activated carbon filter press to filter, the filter cake is squeezed dry, and the filtrate is collected in an acid adjustment kettle to adjust acid to a pH value less than 1.0, the feed liquid is pumped into a filter press to filter, and the filter cake is squeezed dry to obtain
- the refined 2,4-dinitrophenol filter cake has a filter cake yield of 30% (the yield refers to the mass percentage of the filter cake to the mass of the mother liquor recovered by hydrolysis, the same below).
- the refined 2,4-dinitrophenol filter cake was detected and analyzed, and the results are shown in Table 1. It can be seen from Table 1 that the by-product meets the requirements of relevant national product index standards and has good environmental friendliness from the test results of product appearance and purity.
- the product should be kept away from fire, heat source and flammable during production and storage. , Combustibles, avoid mixing with oxidants and alkalis.
- This product can be sold as a by-product and used as a raw material for the production of coating intermediates.
- a kind of production method of dye disperse blue B56# by utilizing sodium sulfite to treat 1-aminoanthraquinone DMF residue to purify and produce mixed nitrate, then the mixed nitrate is sequentially passed through mononitration, mononitration refining, condensation, dinitration, hydrolysis, reduction and In the process of bromination transformation, the product disperse blue B56# is finally obtained; the mother liquor recovered by hydrolysis is reprocessed to recover the by-product 2,4-dinitrophenol.
- the reprocessing of the recovered mother liquor by hydrolysis specifically includes the following steps:
- step (2) Add activated carbon to the solution of step (1), stir and decolorize for 1h; the ratio of the consumption of activated carbon to the quality of the hydrolysis recovery mother liquor is 1:3;
- the material is pumped into an activated carbon filter press to filter, the filter cake is squeezed dry, and the filtrate is collected in an acid adjustment kettle to adjust acid to a pH value less than 1.0, the feed liquid is pumped into a filter press to filter, and the filter cake is squeezed dry to obtain
- the refined 2,4-dinitrophenol filter cake has a filter cake yield of 20%.
- the refined 2,4-dinitrophenol filter cake was detected and analyzed, which met the requirements of relevant national product index standards.
- a kind of production method of dye disperse blue B56# by utilizing sodium sulfite to treat 1-aminoanthraquinone DMF residue to purify and produce mixed nitrate, then the mixed nitrate is sequentially passed through mononitration, mononitration refining, condensation, dinitration, hydrolysis, reduction and In the process of bromination transformation, the product disperse blue B56# is finally obtained; the mother liquor recovered by hydrolysis is reprocessed to recover the by-product 2,4-dinitrophenol.
- the reprocessing of the recovered mother liquor by hydrolysis specifically includes the following steps:
- step (2) Add activated carbon to the solution of step (1), stir and decolorize for 1h; the ratio of the consumption of activated carbon to the quality of the mother liquor recovered by hydrolysis is 1:5;
- the material is pumped into an activated carbon filter press to filter, the filter cake is squeezed dry, and the filtrate is collected in an acid adjustment kettle to adjust acid to a pH value less than 1.0, the feed liquid is pumped into a filter press to filter, and the filter cake is squeezed dry to obtain
- the refined 2,4-dinitrophenol filter cake has a filter cake yield of 35%.
- the refined 2,4-dinitrophenol filter cake was detected and analyzed, which met the requirements of relevant national product index standards.
- a kind of production method of dye disperse blue B56# by utilizing sodium sulfite to treat 1-aminoanthraquinone DMF residue to purify and produce mixed nitrate, then the mixed nitrate is sequentially passed through mononitration, mononitration refining, condensation, dinitration, hydrolysis, reduction and In the process of bromination transformation, the product disperse blue B56# is finally obtained; the mother liquor recovered by hydrolysis is reprocessed to recover the by-product 2,4-dinitrophenol.
- the reprocessing of the recovered mother liquor by hydrolysis specifically includes the following steps:
- step (2) Add activated carbon to the solution of step (1), stir and decolorize for 1h; the ratio of the consumption of activated carbon to the quality of the hydrolysis recovery mother liquor is 1:3;
- the material is pumped into an activated carbon filter press to filter, the filter cake is squeezed dry, and the filtrate is collected in an acid adjustment kettle to adjust acid to a pH value less than 1.0, the feed liquid is pumped into a filter press to filter, and the filter cake is squeezed dry to obtain
- the refined 2,4-dinitrophenol filter cake has a filter cake yield of 40%.
- the refined 2,4-dinitrophenol filter cake was detected and analyzed, which met the requirements of relevant national product index standards.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明公开了一种染料分散蓝B56#的生产方法,属于化工染料技术领域。通过利用亚硫酸钠处理1-氨基蒽醌DMF残渣提纯生产混硝,然后再将混硝依次通过一硝化、一硝化精制、缩合、二硝化、水解、还原和溴化转型过程,最后得到产物分散蓝B56#;对水解回收母液进行再处理回收副产品2,4-二硝基苯酚。本发明分散蓝B56#滤饼水解反应过程中产生了2,4-二硝基苯酚钠盐,2,4-二硝基苯酚钠盐溶解在水解回收母液中,为有效利用其中的有效成分,减少三废排放量,通过酸化、过滤生产副产品2-4-二硝基苯酚,该副产品检测均符合标准,可用作生产涂料中间体的企业原料。
Description
本发明属于化工染料技术领域,具体涉及一种染料分散蓝B56#的生产方法。
现有的1-氨基蒽醌生产线中一次精制过程中产生DMF蒸馏残渣量非常大,该废渣属于危险废物(HW12),现有处置方式为送厂内焚烧炉焚烧处理,这样既浪费了大量原料,也带来了环境污染。所以通常选择将该固体残渣用于染料分散蓝B56#的生产中,生产过程会使用到大量的洗涤水,洗涤水中会存在大量的副产品,如果不经处理就排放必然带来更大的水污染,还有很大的原料浪费,为了节约生产成本和保护环境,应该寻找一种绿色环保节约的染料分散蓝B56#的生产方法和生产过程。
发明内容
针对现有技术中存在的问题,本发明要解决的技术问题在于提供一种染料分散蓝B56#的生产方法,有效利用水解回收母液中的有效成分,减少三废排放量,通过酸化、过滤生产副产品2-4-二硝基苯酚。
为了解决上述问题,本发明所采用的技术方案如下:
一种染料分散蓝B56#的生产方法,通过利用亚硫酸钠处理1-氨基蒽醌DMF残渣提纯生产混硝,然后再将混硝依次通过一硝化、一硝化精制、缩合、二硝化、水解、还原和溴化转型过程,最后得到产物分散蓝B56#;对水解回收母液进行再处理回收副产品2,4-二硝基苯酚。
所述染料分散蓝B56#的生产方法,所述水解回收母液再处理具体包括以下步骤:
(1)将水解回收母液加入精制釜中,室温下缓慢加入硫酸;
(2)向步骤(1)的溶液中加入活性碳,搅拌脱色0.5~1h;
(3)将物料泵入活性炭压滤机进行过滤,滤饼挤干,滤液收集至调酸釜调酸,将料液泵入压滤机进行过滤,滤饼挤干,得到精制后的2,4-二硝基苯酚滤饼。该副产品生产过程中涉及的反应方程式主要为:
所述染料分散蓝B56#的生产方法,对精制后的2,4-二硝基苯酚滤饼进行产品检测若不合格,将2,4-二硝基苯酚滤饼再次加入精制釜中,加入底水,调节pH值为6~7,然后重复步骤(2)和(3)。
所述染料分散蓝B56#的生产方法,所述步骤(1)加入硫酸调节溶液至pH值为4~7。
所述染料分散蓝B56#的生产方法,所述步骤(3)滤液加入调酸釜调节pH≤1.0。
所述染料分散蓝B56#的生产方法,所述步骤(1)反应温度为60~70℃,反应时间为0.5~1h。
所述染料分散蓝B56#的生产方法,所述硫酸的质量分数为90%~98%,所述硫酸的用量为水解回收母液质量的40%~50%。
所述染料分散蓝B56#的生产方法,所述步骤(2)中活性炭的用量与水解回收母液质量之比为1:3~1:5。
有益效果:与现有的技术相比,本发明的优点包括:
本发明分散蓝B56#滤饼水解反应过程中产生了2,4-二硝基苯酚钠盐,2,4-二硝基苯酚钠盐溶解在水解回收母液中,为有效利用其中的有效成分,减少三废排放量,通过酸化、过滤生产副产品2-4-二硝基苯酚,该副产品检测均符合标准,可用作生产涂料中间体的企业原料。
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合具体实施例对本发明的具体实施方式做详细的说明。
实施例1
一种染料分散蓝B56#的生产方法,通过利用亚硫酸钠处理1-氨基蒽醌DMF残渣提纯生产混硝,然后再将混硝依次通过一硝化、一硝化精制、缩合、二硝化、水解、还原和溴化转型过程,最后得到产物分散蓝B56#;对水解回收母液进行再处理回收副产品2,4-二硝基苯酚。
水解回收母液再处理具体包括以下步骤:
(1)将水解回收母液加入精制釜中,室温下缓慢加入质量分数为98%的硫酸调节溶液至pH值为5,硫酸用量为水解回收母液质量的45%;然后调节反应温度为65℃,反应时间为1h;
(2)向步骤(1)的溶液中加入活性碳,搅拌脱色0.8h;活性炭的用量与水解回收母液质量之比为1:3;
(3)将物料泵入活性炭压滤机进行过滤,滤饼挤干,滤液收集至调酸釜调酸至pH值小于1.0,将料液泵入压滤机进行过滤,滤饼挤干,得到精制后的2,4-二硝基苯酚滤饼,滤饼收率为30%(该收率指的是滤饼质量占水解回收母液质量的质量百分比,下同)。对精制后的2,4-二硝基苯酚滤饼进行检测分析,结果如表1所示。由表1可知,从产品外观、纯度等各方面检测结果显示,该副产品符合相关国家产品指标标准要求,具有良好的环境友好性,该产品生产及储存过程中应远离火种、热源,远离易燃、可燃物,避免与氧化剂、碱类物质混存,该产品可作为副产品外售用作生产涂料中间体的企业原料。
表1 2-4-二硝基苯酚检验参数对照表
实施例2
一种染料分散蓝B56#的生产方法,通过利用亚硫酸钠处理1-氨基蒽醌DMF残渣提纯生产混硝,然后再将混硝依次通过一硝化、一硝化精制、缩合、二硝化、水解、还原和溴化转型过程,最后得到产物分散蓝B56#;对水解回收母液进行再处理回收副产品2,4-二硝基苯酚。
水解回收母液再处理具体包括以下步骤:
(1)将水解回收母液加入精制釜中,室温下缓慢加入质量分数为90%的硫酸调节溶液至pH值为7,硫酸用量为水解回收母液质量的50%;然后调节反应温度为60℃,反应时间为0.5h;
(2)向步骤(1)的溶液中加入活性碳,搅拌脱色1h;活性炭的用量与水解回收母液质量之比为1:3;
(3)将物料泵入活性炭压滤机进行过滤,滤饼挤干,滤液收集至调酸釜调酸至pH值小于1.0,将料液泵入压滤机进行过滤,滤饼挤干,得到精制后的2,4-二硝基苯酚滤饼,滤饼收率为20%。对精制后的2,4-二硝基苯酚滤饼进行检测分析,符合相关国家产品指标标准要求。
实施例3
一种染料分散蓝B56#的生产方法,通过利用亚硫酸钠处理1-氨基蒽醌DMF残渣提纯生产混硝,然后再将混硝依次通过一硝化、一硝化精制、缩合、二硝化、水解、还原和溴化转型过程,最后得到产物分散蓝B56#;对水解回收母液进行再处理回收副产品2,4-二硝基苯酚。
水解回收母液再处理具体包括以下步骤:
(1)将水解回收母液加入精制釜中,室温下缓慢加入质量分数为95%的硫酸调节溶液至pH值为5,硫酸用量为水解回收母液质量的45%;然后调节反应温度为70℃,反应时间为1h;
(2)向步骤(1)的溶液中加入活性碳,搅拌脱色1h;活性炭的用量与水解回收母液质量之比为1:5;
(3)将物料泵入活性炭压滤机进行过滤,滤饼挤干,滤液收集至调酸釜调酸至pH值小于1.0,将料液泵入压滤机进行过滤,滤饼挤干,得到精制后的2,4-二硝基苯酚滤饼,滤饼收率为35%。对精制后的2,4-二硝基苯酚滤饼进行检测分析,符合相关国家产品指标标准要求。
实施例4
一种染料分散蓝B56#的生产方法,通过利用亚硫酸钠处理1-氨基蒽醌DMF残渣提纯生产混硝,然后再将混硝依次通过一硝化、一硝化精制、缩合、二硝化、水解、还原和溴化转型过程,最后得到产物分散蓝B56#;对水解回收母液进行再处理回收副产品2,4-二硝基苯酚。
水解回收母液再处理具体包括以下步骤:
(1)将水解回收母液加入精制釜中,室温下缓慢加入质量分数为98%的硫酸调节溶液至pH值为5,硫酸用量为水解回收母液质量的50%;然后调节反应温度为70℃,反应时间为1h;
(2)向步骤(1)的溶液中加入活性碳,搅拌脱色1h;活性炭的用量与水解回收母液质量之比为1:3;
(3)将物料泵入活性炭压滤机进行过滤,滤饼挤干,滤液收集至调酸釜调酸至pH值小于1.0,将料液泵入压滤机进行过滤,滤饼挤干,得到精制后的2,4-二硝基苯酚滤饼,滤饼收率为40%。对精制后的2,4-二硝基苯酚滤饼进行检测分析,符合相关国家产品指标标准要求。
Claims (8)
- 一种染料分散蓝B56#的生产方法,其特征在于,通过利用亚硫酸钠处理1-氨基蒽醌DMF残渣提纯生产混硝,然后再将混硝依次通过一硝化、一硝化精制、缩合、二硝化、水解、还原和溴化转型过程,最后得到产物分散蓝B56#;对水解回收母液进行再处理回收副产品2,4-二硝基苯酚。
- 根据权利要求1所述染料分散蓝B56#的生产方法,其特征在于,所述水解回收母液再处理具体包括以下步骤:(1)将水解回收母液加入精制釜中,室温下缓慢加入硫酸;(2)向步骤(1)的溶液中加入活性碳,搅拌脱色0.5~1h;(3)将物料泵入活性炭压滤机进行过滤,滤饼挤干,滤液收集至调酸釜调酸,将料液泵入压滤机进行过滤,滤饼挤干,得到精制后的2,4-二硝基苯酚滤饼。
- 根据权利要求2所述染料分散蓝B56#的生产方法,其特征在于,对精制后的2,4-二硝基苯酚滤饼进行产品检测若不合格,将2,4-二硝基苯酚滤饼再次加入精制釜中,加入底水,调节pH值为6~7,然后重复步骤(2)和(3)。
- 根据权利要求2所述染料分散蓝B56#的生产方法,其特征在于,所述步骤(1)加入硫酸调节溶液至pH值为4~7。
- 根据权利要求2所述染料分散蓝B56#的生产方法,其特征在于,所述步骤(3)滤液加入调酸釜调节PH≤1.0。
- 根据权利要求2所述染料分散蓝B56#的生产方法,其特征在于,所述步骤(1)反应温度为60~70℃,反应时间为0.5~1h。
- 根据权利要求2所述染料分散蓝B56#的生产方法,其特征在于,所述硫酸的质量分数为90%~98%,所述硫酸的用量为水解回收母液质量的40%~50%。
- 根据权利要求2所述染料分散蓝B56#的生产方法,其特征在于,所述步骤(2)中活性炭的用量与水解回收母液质量之比为1:3~1:5。
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