CN106632116B - 一种水溶性重质碳酸钙粉体荧光增白剂及其制备方法和应用 - Google Patents
一种水溶性重质碳酸钙粉体荧光增白剂及其制备方法和应用 Download PDFInfo
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 80
- 239000000843 powder Substances 0.000 title claims abstract description 53
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 40
- 239000006081 fluorescent whitening agent Substances 0.000 title claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 16
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000005282 brightening Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 abstract description 5
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- 230000001681 protective effect Effects 0.000 abstract 1
- 239000002253 acid Substances 0.000 description 13
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- 239000007864 aqueous solution Substances 0.000 description 10
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- YWFWDNVOPHGWMX-UHFFFAOYSA-N n,n-dimethyldodecan-1-amine Chemical compound CCCCCCCCCCCCN(C)C YWFWDNVOPHGWMX-UHFFFAOYSA-N 0.000 description 8
- 241000276489 Merlangius merlangus Species 0.000 description 7
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 7
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 7
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- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 description 4
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 229950000244 sulfanilic acid Drugs 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 239000005457 ice water Substances 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical compound [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 150000002500 ions Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- -1 weaving Substances 0.000 description 2
- 230000002087 whitening effect Effects 0.000 description 2
- MAUMSNABMVEOGP-UHFFFAOYSA-N (methyl-$l^{2}-azanyl)methane Chemical compound C[N]C MAUMSNABMVEOGP-UHFFFAOYSA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- HDWLUGYOLUHEMN-UHFFFAOYSA-N Dinobuton Chemical compound CCC(C)C1=CC([N+]([O-])=O)=CC([N+]([O-])=O)=C1OC(=O)OC(C)C HDWLUGYOLUHEMN-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 241000425573 Talanes Species 0.000 description 1
- NCSHGROOCJHAFK-UHFFFAOYSA-N [Cl].N#CC#N Chemical compound [Cl].N#CC#N NCSHGROOCJHAFK-UHFFFAOYSA-N 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000002649 leather substitute Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005829 trimerization reaction Methods 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
- C07D251/70—Other substituted melamines
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
本发明公开一种水溶性重质碳酸钙粉体荧光增白剂,所述的水溶性重质碳酸钙粉体荧光增白剂为以下结构式1:本发明的目的在于提供一种水溶性重质碳酸钙粉体荧光增白剂及其制备方法和应用,该方法简单,原材料价格低廉,工艺绿色环保。采用本发明的荧光增白剂能有效增白、增亮碳酸钙粉体,还兼具表面改性作用。
Description
技术领域
本发明涉及荧光增白剂技术领域,具体涉及一种水溶性重质碳酸钙粉体荧光增白剂及其制备方法和应用。
背景技术
我国在“十二五”新材料发展规划中将开发与资源、环境协调的新材料作为主要考核指标,通过开发新材料解决资源短缺问题。我国已经形成了比较完善的材料科技体系,在某些新材料领域内具有明显的资源优势和技术优势,但总体自主创新能力还比较薄弱,具有自主知识产权的新材料产品及技术还比较少,尤其是在重质碳酸钙粉体荧光增白材料方面创新性不足。
荧光增白剂具有很高的光量子产率,对被处理的基质能有效地增白、増艳。荧光增白剂分子具有较大的共轭体系,能够吸收波长范围在300~400nm左右的紫外光,并发射出波长范围在420~450nm左右的蓝色荧光,从而弥补了基质中由于蓝光缺失而造成的视觉上的泛黄。通过弥补蓝光使人感到被处理的基质更亮洁、更鲜艳。荧光增白剂被广泛地用于造纸、纺织、洗涤剂、塑料、油墨、皮革、紫外吸收剂、显影剂等诸多领域,市场需求巨大。
重质碳酸钙作为最大的无机填料,由于原料广、价格低、无毒等优点,被广泛应用于电缆料、合成革、聚乙烯薄膜,泡沫塑料、塑料管材、纸张等制品的填充料或原料。重质碳酸钙粉体作为最大填充材料,人们对其白度和光泽度均有较高要求,市场上有众多塑料、造纸和洗涤剂等专用荧光增白剂,但重质碳酸钙等粉体荧光增白剂却不多见,市场需求迫切、巨大。
碳酸粉体表面具有游离钙离子和羟基,市场上现有的荧光增白剂产品很难有效与粉体表面离子或基团发生有效键合或表面吸附,因此缺乏能有效增白、增亮重质碳酸钙粉体的荧光增白材料。
发明内容
针对上述不足,本发明的目的在于提供一种水溶性重质碳酸钙粉体荧光增白剂及其制备方法和应用,该水溶性钙粉体荧光增白剂合成方法简单,原材料价格低廉,工艺绿色环保。通过测试水溶性酸荧光增白剂的光学性能和对重质碳酸钙粉体荧光增白效果,可以明显看出该水溶性荧光增白剂具有较强的紫外吸收性能、对重钙粉体具有较强的键合能力和显著的增白、增亮作用,处理后的碳酸钙粉体具有较高的流动性和分散性,兼具辅助表面改性作用,是一种高性能重钙粉体荧光增白、表面改性材料,具有极大的推广和应用空间。
具体来说,本发明的方案为:一种水溶性重质碳酸钙粉体荧光增白剂,所述的水溶性重质碳酸钙粉体荧光增白剂为以下结构式1:
同时本发明还公开了上述的水溶性重质碳酸钙粉体荧光增白剂的制备方法,包括以下步骤:
步骤1:将4,4'-二氨基二苯乙烯-2,2'-二磺酸水溶液加入到三聚氯氰水溶液中,在0~5℃条件下搅拌反应一段时间;
步骤2:调节步骤1的混合物pH值为3~4,然后加入十四烷基二甲基叔胺溶液,在30~40℃的条件下反应一段时间;
步骤3:向步骤2的混合物中加入对氨基苯磺酸并维持反应体系pH为8~9,在80~90℃的条件下反应一段时间;
步骤4:冷却后加入无机盐使水溶性重质碳酸钙粉体荧光增白剂析出并收集;
其中,三聚氯氰、4,4'-二氨基二苯乙烯-2,2'-二磺酸、十四烷基二甲基叔胺、对氨基苯磺酸的物质的量的比例为:1.9~2.1:0.9~1.1:1.8~2.1:1.8~2.2。
在上述的水溶性重质碳酸钙粉体荧光增白剂的制备方法中,所述的步骤1中,三聚氯氰水溶液中,每19~21mmol三聚氯氰对应200~250mL水;
4,4'-二氨基二苯乙烯-2,2'-二磺酸水溶液中,每9~11mmol摩尔4,4'-二氨基二苯乙烯-2,2'-二磺酸对应195~205mL水。
在上述的水溶性重质碳酸钙粉体荧光增白剂的制备方法中,所述的4,4'-二氨基二苯乙烯-2,2'-二磺酸水溶液的pH值为7~8。
在上述的水溶性重质碳酸钙粉体荧光增白剂的制备方法中,pH值通过Na2CO3调控。
在上述的水溶性重质碳酸钙粉体荧光增白剂的制备方法中,所述的十四烷基二甲基叔胺溶液中每18~21mmol十四烷基二甲基叔胺对应9~11mL有机溶剂二甲基甲酰胺。
在上述的水溶性重质碳酸钙粉体荧光增白剂的制备方法中,所述的步骤1的反应时间为1.5~2h;步骤2的反应时间为9~10h;步骤3的反应时间为7~8h。
在上述的水溶性重质碳酸钙粉体荧光增白剂的制备方法中,步骤4中的无机盐为氯化钠。
在上述的水溶性重质碳酸钙粉体荧光增白剂的制备方法中,所述的步骤1中,4,4'-二氨基二苯乙烯-2,2'-二磺酸水溶液以滴加的形式加入到三聚氯氰水溶液中;
所述的步骤2中十四烷基二甲基叔胺溶液以滴加的形式加入到步骤1的混合物中。
另外,本发明还提供一种如上述的水溶性重质碳酸钙粉体荧光增白剂的用途,其用于重质碳酸钙粉体荧光增白和表面改性的应用。
与现有技术相比,本发明提供的技术方案有以下优点:
1.本发明荧光增白剂产品含有四个水溶性磺酸基,水溶性较好,能与碳酸钙粉体表面离子发生有效键合,结合牢固性高。
2.本发明产品具有较强的紫外吸收性能,可以明显的增白、增亮重质碳酸钙粉体。
3.本发明荧光增白剂产品对重钙粉体具表面改性作用,处理后的粉体具有较好的流动性和分散性。
附图说明
图1为实施例1的水溶性重质碳酸钙粉体荧光增白剂的核磁氢谱;
图2为实施例1的水溶性重质碳酸钙粉体荧光增白剂水溶液的光学性能测试中紫外吸收谱图。
具体实施例
下面结合具体实施方式,对本发明的权利要求做进一步的详细说明,但不构成对本发明的任何限制,任何在本发明权利要求范围内所做的有限次的修改,仍在本发明的权利要求保护范围内。
实施例1
20mmol三聚氯氰加到200mL冰水中,冰浴。而后滴加10mmol 4,4'-二氨基二苯乙烯-2,2'-二磺酸(DSD酸)与200mL蒸馏水的混合液(加20mmol Na2CO3),搅拌,0~5℃,反应2h。升温至30~40℃,加20mmol Na2CO3。而后滴加20mmol十四烷基二甲基叔胺与10mL二甲基甲酰胺混合液,控温反应10h。升温至80~90℃,加入20mmol对氨基苯磺酸,滴加10%Na2CO3溶液维持体系pH 8~9,控温反应8h。冷却至室温,加入60g氯化钠,搅拌、抽滤,真空干燥得水溶性重质碳酸钙粉体荧光增白剂,收率90%。
实施例2
19mmol三聚氯氰加到250mL冰水中,冰浴。而后滴加11mmol 4,4'-二氨基二苯乙烯-2,2'-二磺酸(DSD酸)与195mL蒸馏水的混合液(加20mmol Na2CO3),搅拌,0~5℃,反应2h。升温至30~40℃,加20mmol Na2CO3。而后滴加21mmol十四烷基二甲基叔胺与9mL二甲基甲酰胺混合液,控温反应10h。升温至80~90℃,加入22mmol对氨基苯磺酸,滴加10%Na2CO3溶液维持体系pH 8~9,控温反应8h。冷却至室温,加入60g氯化钠,搅拌、抽滤,真空干燥得水溶性重质碳酸钙粉体荧光增白剂,收率88%。
实施例3
21mmol三聚氯氰加到225mL冰水中,冰浴。而后滴加9mmol 4,4'-二氨基二苯乙烯-2,2'-二磺酸(DSD酸)与205mL蒸馏水的混合液(加20mmol Na2CO3),搅拌,0~5℃,反应2h。升温至30~40℃,加20mmol Na2CO3。而后滴加18mmol十四烷基二甲基叔胺与11mL二甲基甲酰胺混合液,控温反应10h。升温至80~90℃,加入18mmol对氨基苯磺酸,滴加10%Na2CO3溶液维持体系pH 8~9,控温反应8h。冷却至室温,加入60g氯化钠,搅拌、抽滤,真空干燥得水溶性重质碳酸钙粉体荧光增白剂,收率89%。
物质结构测试
本发明采用核磁氢谱法对本发明实施例1产物进行物质结构测试,核磁氢谱图如图1所示:
氢谱数据(400MHz;DMSO-d6,δ):0.84(6H,CH3),1.22-1.56(48H,(CH2)12),2.71(12H,(CH3)2N),3.10(4H,CH2),7.56-8.03(14H,ArH),7.67(2H,CH=CH),9.21(2H,NH),10.74(2H,NH)。
光学性能测试
本发明采用紫外吸收光谱法对本发明实施例1产物进行光学性能测试,紫外吸收谱图如图2所示:
紫外-可见光谱可以有效地测试荧光增白剂分子的共轭体系。水溶性重质碳酸钙粉体荧光增白剂配制成浓度为10-6mol/L的水溶液进行光学性能测试。测试结果表明,水溶性荧光增白剂有较强的紫外吸收,最大反式吸收峰位于346nm。
增白性能测试
配制水溶性重质碳酸钙粉体荧光增白剂质量浓度为0.01~0.03%的水溶液100mL,处理100g不同粒度和白度的重质碳酸钙粉体。具体做法如下:将不同品质的重质碳酸钙粉体放入适量上述浓度的溶液中,室温搅拌30min,抽干,干燥,即可得到高白、高亮重质碳酸钙粉体。实验结果证实,水溶性重质碳酸钙粉体荧光增白剂对不同品质的重钙粉体有显著的增白效果,在浓度为0.02%时,对400~3000目,白度为90~95的重钙粉体增加白度值1~2.5之间。增白处理后的粉体具有较好的分散性和流动性。水溶性荧光增白剂是一类高性能重钙粉体增白剂,兼具表面改性作用,具有重要的使用价值和应用前景。
以上所述的仅为本发明的较佳实施例,凡在本发明的精神和原则范围内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (2)
1.一种水溶性重质碳酸钙粉体荧光增白剂,其特征在于,所述的水溶性重质碳酸钙粉体荧光增白剂为以下结构式1:
2.一种如权利要求1所述的水溶性重质碳酸钙粉体荧光增白剂的用途,其特征在于,其用于重质碳酸钙粉体荧光增白和表面改性的应用。
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