CN109679366A - 蒽醌型羧酸酯分散染料及其制备方法 - Google Patents
蒽醌型羧酸酯分散染料及其制备方法 Download PDFInfo
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- 150000007942 carboxylates Chemical class 0.000 title claims abstract description 44
- 239000000986 disperse dye Substances 0.000 title claims abstract description 41
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 150000004056 anthraquinones Chemical class 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000975 dye Substances 0.000 claims abstract description 46
- -1 normal-butyl Chemical group 0.000 claims abstract description 10
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims abstract description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims abstract description 3
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 claims abstract description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims abstract description 3
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 claims abstract description 3
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 claims abstract description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
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- 239000012065 filter cake Substances 0.000 claims description 7
- CAHGWVAXFJXDNI-UHFFFAOYSA-N 1,4-dichloroanthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C(Cl)=CC=C2Cl CAHGWVAXFJXDNI-UHFFFAOYSA-N 0.000 claims description 6
- IOHPVZBSOKLVMN-UHFFFAOYSA-N 2-(2-phenylethyl)benzoic acid Chemical compound OC(=O)C1=CC=CC=C1CCC1=CC=CC=C1 IOHPVZBSOKLVMN-UHFFFAOYSA-N 0.000 claims description 6
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 6
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- 229940090248 4-hydroxybenzoic acid Drugs 0.000 claims description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical class [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 3
- DNUYOWCKBJFOGS-UHFFFAOYSA-N 2-[[10-(2,2-dicarboxyethyl)anthracen-9-yl]methyl]propanedioic acid Chemical compound C1=CC=C2C(CC(C(=O)O)C(O)=O)=C(C=CC=C3)C3=C(CC(C(O)=O)C(O)=O)C2=C1 DNUYOWCKBJFOGS-UHFFFAOYSA-N 0.000 claims description 2
- IJFXRHURBJZNAO-UHFFFAOYSA-N meta--hydroxybenzoic acid Natural products OC(=O)C1=CC=CC(O)=C1 IJFXRHURBJZNAO-UHFFFAOYSA-N 0.000 claims description 2
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- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical compound [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
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- TVRGPOFMYCMNRB-UHFFFAOYSA-N quinizarine green ss Chemical compound C1=CC(C)=CC=C1NC(C=1C(=O)C2=CC=CC=C2C(=O)C=11)=CC=C1NC1=CC=C(C)C=C1 TVRGPOFMYCMNRB-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
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- 125000004494 ethyl ester group Chemical group 0.000 description 1
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- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
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Classifications
-
- 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
- C09B1/16—Amino-anthraquinones
- C09B1/20—Preparation from starting materials already containing the anthracene nucleus
- C09B1/26—Dyes with amino groups substituted by hydrocarbon radicals
- C09B1/32—Dyes with amino groups substituted by hydrocarbon radicals substituted by aryl groups
-
- 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
- C09B1/02—Hydroxy-anthraquinones; Ethers or esters thereof
- C09B1/06—Preparation from starting materials already containing the anthracene nucleus
- C09B1/14—Dyes containing ether groups
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/16—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dispersed, e.g. acetate, dyestuffs
- D06P1/20—Anthraquinone dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/34—Material containing ester groups
- D06P3/52—Polyesters
- D06P3/54—Polyesters using dispersed dyestuffs
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Organic Chemistry (AREA)
- Coloring (AREA)
Abstract
本发明公开了一种蒽醌型羧酸酯分散染料,分子结构中含有羧酸酯基团,其结构通式为:
Description
技术领域
本发明涉及一种蒽醌型羧酸酯分散染料及其制备方法。
背景技术
我国分散染料的产量世界第一,但是目前染料制造企业普遍存在品种陈旧、技术落后等问题,导致国内分散染料的利润率偏低,而同时环保压力的不断增大,使得整个纺织行业的发展面临困境。开发新型高牢度染料和提升现有染料生产技术,增加染料的技术含量,将是染料行业发展的必由之路。发展低污型染料,减少染料制造、应用、后处理过程中有害化学药品的使用,从根本上解决印染废水毒性大,以及COD、BOD畸高、难以处理等行业难题是染料制造与印染行业未来发展的重中之重。
传统染料制造企业在生产、使用过程中不可避免会产生三废(废水、废渣、废气)。目前市场上所用的分散染料在染色后,必须经过还原清洗去除织物表面浮色,以提高织物的各项色牢度。由于还原清洗过程中使用大量保险粉和浓度较高的强碱溶液,处理后的还原液中存在着高浓度的未反应保险粉、氢氧化钠以及具有潜在致癌性或诱变性的芳胺化合物,将这些废水排入江河中会对水体造成严重污染。此外,保险粉在储存和使用过程中也存在着安全隐患,保险粉吸潮后容易自燃,存在火灾隐患;在使用过程中还会逸出大量刺激性气体,加重环境污染,危害健康。
申请号为201510523507X的发明《杂环可碱洗羧酸乙酯型分散染料及其制备方法》选取现有的含氰基的商品分散染料为原料,采用醇解法这一单元反应将氰基转化为羧酸酯基,从而制得羧酸酯型分散染料,该方法虽然为一步法,但将染料中的氰基转化为羧酸酯基不仅反应条件较为苛刻,而且会造成耐日晒牢度的下降(一般会导致下降1-2级),劣化染料某些应用性能。
以含有氰基的C.I.分散橙25为原料,无水乙醇为溶剂和反应物,浓硫酸为催化剂,利用氰基醇解反应制得羧酸酯型偶氮分散染料D1。
C.I.分散橙25与D1分别经过砂磨和对涤纶染色后,获得的染色织物采用国家标准《纺织品色牢度试验耐光色牢度日光》(GB/T 8426-1998)测定耐光色牢度,C.I.分散橙25染色布样的耐光色牢度为6级,D1染色布样的耐光色牢度为4-5级。由此可见,氰基被酯基取代劣化了染料的耐光色牢度性能。
发明内容
本发明要解决的技术问题是提供一种蒽醌型羧酸酯分散染料及其制备方法,该分散染料具有应用于涤纶染色时上染率高、色牢度好,在后处理时具有易碱洗、免用保险粉等特点。
为了解决上述技术问题,本发明提供一种蒽醌型羧酸酯分散染料,其分子结构中含有羧酸酯基团,其结构通式如下:
式中:R为乙基、正丙基、异丙基、正丁基、异丁基、特丁基、正己基等;X为NH或O。
作为本发明的蒽醌型羧酸酯分散染料的进一步改进,该分散染料的结构式为以下任一:
本发明还同时提供了上述蒽醌型羧酸酯分散染料的制备方法,包括如下步骤:
1)、将1,4-二氯蒽醌、苯甲酸类化合物、氧化镁、氧化铜、氢氧化钾、醇水溶液混合后,置于釜中于150±20℃反应20±2小时;得到羧酸中间体;
1,4-二氯蒽醌:苯甲酸类化合物=1:5~6的摩尔比(优选1:5.6);
每0.025mol 1,4-二氯蒽醌配用1.6±0.2g氧化镁、0.4±0.05g氧化铜、8.0±1g氢氧化钾;
所述苯甲酸类化合物为氨基苯甲酸类化合物或羟基苯甲酸类化合物;
2)、在步骤1)所得的羧酸中间体中加入无水醇类物质、硫酸(浓硫酸),回流反应1.5~2.5小时(薄层色谱法检测反应终点);然后蒸馏,直至无水醇类物质被蒸出(全部蒸出);接着依次进行以下步骤:先降温至室温,再调pH为中性,然后于室温下静置1±0.2h,最后抽滤,所得滤饼烘干(80℃烘干至恒重),得蒽醌型羧酸酯染料;
每0.01mol的羧酸中间体配用4±0.2g的硫酸(浓硫酸)。
作为本发明的蒽醌型羧酸酯分散染料的制备方法的改进:
氨基苯甲酸类化合物为邻氨基苯甲酸、间氨基苯甲酸、对氨基苯甲酸;
羟基苯甲酸类化合物为邻羟基苯甲酸、间羟基苯甲酸、对羟基苯甲酸。
作为本发明的蒽醌型羧酸酯分散染料的制备方法的进一步改进:
所述步骤1)的醇水溶液为异丁醇:水=1:13~17(优选1:15)体积比的混合液;
每0.025mol 1,4-二氯蒽醌配用60~70ml的醇水溶液。
作为本发明的蒽醌型羧酸酯分散染料的制备方法的进一步改进:
步骤1)中,每0.025mol 1,4-二氯蒽醌反应结束后所得的反应液先用500±50ml水稀释,再用10±1ml硫酸(浓硫酸)酸化;静置冷却至室温后,过滤,用水洗涤滤饼,干燥至恒重,得羧酸中间体。
作为本发明的蒽醌型羧酸酯分散染料的制备方法的进一步改进,所述步骤2)中:
无水醇类物质为乙醇、叔丁醇;
每0.01mol的羧酸中间体配用40~60mL的无水醇类物质。
作为本发明的蒽醌型羧酸酯分散染料的制备方法的进一步改进,步骤2)中:利用饱和碳酸钠溶液调节pH。
在本发明中,浓硫酸是指浓度为98%的硫酸。
本发明的反应式如下:
本发明的蒽醌型羧酸酯分散染料的制备方法,选取制备的含羧酸基蒽醌中间体(即,步骤1)制备所得的羧酸中间体)为原料,采用酯化法制得羧酸酯型分散染料。染料制备过程中所选取的反应原料易得、低毒,并且合成路线短、反应转化率高,能够有效减少有害物质及三废的产生,实现绿色生产。
即,本发明是以简单的取代蒽醌为原料,先制备羧酸染料,再通过与醇直接酯化的一步法合成羧酸酯染料,从羧酸染料转化为羧酸酯只需要一步反应,反应条件更加温和。
本发明开发的蒽醌型羧酸酯分散染料有良好的染色性能,应用于涤纶染色时上染率高、色牢度好,在PET纤维染色后处理时,只需经较稀的碱性溶液处理纤维,使染料酯基发生水解,生成含有水溶性基团的羧酸染料和低毒的醇类物质,并且生成的羧酸染料可通过酸化等方法回收循环使用。该法不仅消除了保险粉的使用,而且有效降低了废水的处理难度。
蒽醌型羧酸酯分散染料用于PET疏水性聚酯纤维的染色,其染色工艺为:取本发明的羧酸酯染料0.5~2g、分散剂NNO 0.5~2g、锆珠(直径1~2mm)10~40g、水20~60mL加入砂磨机中砂磨4~8小时,砂磨结束后,经细尼龙滤布过滤、收集染料分散液并定容于250mL容量瓶,得染料色浆;按0.5~2%的色度要求移取分散染料色浆,按浴比1:30~50加入水后转移至染色杯中,加入欲染色的PET织物放入高温高压染色仪中,按2℃/min的升温速度快速升温至90℃,再以1℃/min缓慢升温至130℃,保温1小时后降至室温,取出染色布样,洗涤,分别吸取染色前后染液,用紫外-可见分光光度计于最大吸收波长(λmax)处测得吸光度,利用朗伯-比尔定律求解染料的上染率。
本发明的蒽醌型羧酸酯分散染料,在染料结构中引入极性强的羧酸酯基团,能够提高染料在聚酯纤维上的亲和力和耐升华牢度,并且具有优异的可碱洗性能,从而具有广阔的应用前景。
综上所述,本发明所开发的染料,生产过程中所选取的反应原料易得、低毒,并且合成路线短、反应转化率高,能够有效减少有害物质及三废的产生,实现绿色生产。应用于涤纶染色时上染率高、色牢度好,在后处理时易碱洗、水解产物低毒、水解染料易回收并且可以循环利用。因此,其易洗、低毒、低污等诸多优势能够有效解决分散染料制造和印染过程中废水COD、BOD畸高等行业难题。
具体实施方式
下面结合具体实施例对本发明进行进一步描述,但本发明的保护范围并不仅限于此:
实施例1、一种蒽醌型羧酸酯分散染料的制备方法,依次进行以下步骤:
1)、以1,4-二氯蒽醌(0.025mol)为原料,将其与对氨基苯甲酸(18.5g,0.14mol)、氧化镁(1.6g)、氧化铜(0.4g)、氢氧化钾(8.0g)、水(60ml)、异丁醇(4ml)混合后置于釜中于150℃反应20小时。反应结束后,反应液用500ml水稀释,再用10ml浓硫酸(98%)酸化。静置冷却至室温后,过滤并用水洗涤滤饼(直至洗涤液的pH为中性),洗涤后的滤饼于80℃干燥至恒重;得到羧酸中间体A1。
2)、在三口烧瓶中加入4.8g(0.01mol)羧酸中间体A1、50mL乙醇(无水乙醇)、4g浓硫酸,回流约2h(薄层色谱法检测反应终点),然后进行蒸馏,当乙醇全部蒸出后则反应结束,并把反应液移至烧杯中待温度降至室温后用饱和碳酸钠滴加使pH调为中性后在室温下静置1h,最后进行抽滤;将滤饼烘干(80℃)至恒重,得蒽醌型羧酸酯染料B1。
1H NMR(400MHz,DMSO-d6):δ10.2(s,2H),7.80(d,2H),7.72(d,4H),7.55(t,2H),6.57(d,4H),6.50(d,2H),4.29(q,4H),1.30(t,6H);ESI MS(m/z,%):535.17([M+H]+,100)。
实施例2、
1)、对实施例1步骤1)作如下更改:用对羟基苯甲酸代替对氨基苯甲酸,其他条件不变,得到羧酸中间体A2,结构式为
2)、以相同摩尔用量的羧酸中间体A2替代羧酸中间体A1,其余同实施例1步骤2),得蒽醌型羧酸酯染料B2。
1H NMR(400MHz,DMSO-d6):δ7.93(d,4H),7.80(d,2H),7.55(t,2H),7.17(d,2H),7.03(d,4H),4.30(q,4H),1.32(t,6H);ESI MS(m/z,%):537.15([M+H]+,100)。
实施例3、
1)、同实施例1步骤1);
2)、以相同体积用量的叔丁醇替代乙醇,其余等同于实施例1步骤2),得蒽醌型羧酸酯染料B3。
1H NMR(400MHz,DMSO-d6):δ10.3(s,2H),7.81(d,2H),7.74(d,4H),7.57(t,2H),6.57(d,4H),6.50(d,2H),1.40(s,18H);ESI MS(m/z,%):591.20([M+H]+,100)。
实施例4、
1)、同实施例2步骤1);
2)、以相同体积用量的叔丁醇替代乙醇,其余同实施例2步骤2),得蒽醌型羧酸酯染料B4。
1H NMR(400MHz,DMSO-d6):δ7.95(d,4H),7.82(d,2H),7.57(t,2H),7.17(d,2H),7.03(d,4H),1.40(s,18H);ESI MS(m/z,%):593.25([M+H]+,100)。
下面通过实验来说明本发明的蒽醌型羧酸酯分散染料在PET纤维染色中的应用。
实验1、
取实施例1中合成的染料B1 0.5g、分散剂NNO 0.5g、锆珠(直径1mm)10g、水20mL加入砂磨机中砂磨8小时,砂磨结束后,经细尼龙滤布过滤、收集染料分散液并定容于250mL容量瓶,得染料色浆;按2%的色度要求移取分散染料色浆,按浴比1:50加入水后转移至染色杯中,加入欲染色的PET织物放入高温高压染色仪中,按2℃/min的升温速度快速升温至90℃,再以1℃/min缓慢升温至130℃,保温1小时后降至室温,取出染色布样,分别吸取染色前后染液各1mL于10mL容量瓶中,加入丙酮至刻度,用紫外-可见分光光度计于最大吸收波长(λmax)处测得吸光度,利用朗伯-比尔定律求解染料的上染率为95.4%。
将上述染色布样采用国家标准《分散染料染色色光和强度的测定方法》(GB/T2394-1980)后处理方法还原清洗后(还原清洗工艺为:2g/L保险粉,1g/L NaOH,浴比1:50,70℃,15min),其耐水色牢度为4级,耐干摩擦牢度为4级,耐湿摩擦牢度为4-5级,耐升华色牢度4-5级。
此外,采用碱洗法除去PET织物表面的浮色,具体方法如下:染好的样品在0.1g/LNaOH水溶液中70℃下处理15min后,再经热水和冷水多次漂洗;碱洗法处理后,上述样品的耐水色牢度为4-5级,耐干摩擦牢度为4-5级,耐湿摩擦牢度为4-5级,耐升华色牢度4-5级。各项色牢度等于或略高于还原清洗后得到的样品的各项色牢度。
将实施例2~实施例4所得的染料如同上述实验1进行检测,所得结果如表1所述:
表1
根据表1的结果能说明对于本发明的蒽醌型羧酸酯分散染料,碱洗法能够获得优于或等于国标还原碱洗法的色牢度结果,而碱洗法所用碱浓度(0.1g/L NaOH水溶液)远低于还原碱洗(1g/L NaOH水溶液),并且免除了保险粉的使用,对洗涤残液的后处理非常有利。
对比实验1、C.I.溶剂绿3(CAS:128-80-3),结构式为:
将C.I.溶剂绿3、作为原料的1,4-二氯蒽醌,按照上述实验1所述方法进行检测,所得结果如下表2所述。并进行了相应的耐光色牢度的检测,结果如下表2所述。
表2
最后,还需要注意的是,以上列举的仅是本发明的若干个具体实施例。显然,本发明不限于以上实施例,还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形,均应认为是本发明的保护范围。
Claims (8)
1.蒽醌型羧酸酯分散染料,其特征在于:分子结构中含有羧酸酯基团,其结构通式为:
式中:R为乙基、正丙基、异丙基、正丁基、异丁基、特丁基、正己基;X为NH或O。
2.根据权利要求1所述的蒽醌型羧酸酯分散染料,其特征在于该分散染料的结构式为以下任一:
3.如权利要求1或2所述的蒽醌型羧酸酯分散染料的制备方法,其特征在于包括如下步骤:
1)、将1,4-二氯蒽醌、苯甲酸类化合物、氧化镁、氧化铜、氢氧化钾、醇水溶液混合后,置于釜中于150±20℃反应20±2小时;得到羧酸中间体;
1,4-二氯蒽醌:苯甲酸类化合物=1:5~6的摩尔比;
每0.025mol1,4-二氯蒽醌配用1.6±0.2g氧化镁、0.4±0.05g氧化铜、8.0±1g氢氧化钾;
所述苯甲酸类化合物为氨基苯甲酸类化合物或羟基苯甲酸类化合物;
2)、在步骤1)所得的羧酸中间体中加入无水醇类物质、硫酸,回流反应1.5~2.5小时;然后蒸馏,直至无水醇类物质被蒸出;接着依次进行以下步骤:先降温至室温,再调pH为中性,然后于室温下静置1±0.2h,最后抽滤,所得滤饼烘干,得蒽醌型羧酸酯染料;
每0.01mol的羧酸中间体配用4±0.2g的硫酸。
4.根据权利要求3所述的蒽醌型羧酸酯分散染料的制备方法,其特征在于:
氨基苯甲酸类化合物为邻氨基苯甲酸、间氨基苯甲酸、对氨基苯甲酸;
羟基苯甲酸类化合物为邻羟基苯甲酸、间羟基苯甲酸、对羟基苯甲酸。
5.根据权利要求4所述的蒽醌型羧酸酯分散染料的制备方法,其特征在于:
所述步骤1)的醇水溶液为异丁醇:水=1:13~17体积比的混合液;
每0.025mol 1,4-二氯蒽醌配用60~70ml的醇水溶液。
6.根据权利要求4或5所述的蒽醌型羧酸酯分散染料的制备方法,其特征在于:
步骤1)中,每0.025mol1,4-二氯蒽醌反应结束后所得的反应液先用500±50ml水稀释,再用10±1ml硫酸酸化;静置冷却至室温后,过滤,用水洗涤滤饼,干燥至恒重,得羧酸中间体。
7.根据权利要求3所述的蒽醌型羧酸酯分散染料的制备方法,其特征在于所述步骤2)中:
无水醇类物质为乙醇、叔丁醇;
每0.01mol的羧酸中间体配用40~60mL的无水醇类物质。
8.根据权利要求7所述的蒽醌型羧酸酯分散染料的制备方法,其特征在于所述步骤2)中:利用饱和碳酸钠溶液调节pH。
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