CN116444258A - 一种利用钢渣与赤泥制备的发泡陶瓷及其工艺 - Google Patents
一种利用钢渣与赤泥制备的发泡陶瓷及其工艺 Download PDFInfo
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- CN116444258A CN116444258A CN202310422086.6A CN202310422086A CN116444258A CN 116444258 A CN116444258 A CN 116444258A CN 202310422086 A CN202310422086 A CN 202310422086A CN 116444258 A CN116444258 A CN 116444258A
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- Prior art keywords
- red mud
- steel slag
- parts
- prepared
- foamed ceramic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000002893 slag Substances 0.000 title claims abstract description 42
- 239000010959 steel Substances 0.000 title claims abstract description 42
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 30
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002844 melting Methods 0.000 claims abstract description 21
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- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 17
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- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 11
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- KHAVLLBUVKBTBG-UHFFFAOYSA-N dec-9-enoic acid Chemical compound OC(=O)CCCCCCCC=C KHAVLLBUVKBTBG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 35
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 27
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 12
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 12
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- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims description 12
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- 235000012239 silicon dioxide Nutrition 0.000 claims description 12
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 12
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 12
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
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- 239000002202 Polyethylene glycol Substances 0.000 claims description 9
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
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- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims description 9
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- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 6
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 5
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000010008 shearing Methods 0.000 claims description 5
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical group [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 2
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 2
- 229960005055 sodium ascorbate Drugs 0.000 claims description 2
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical group [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 2
- 238000005187 foaming Methods 0.000 abstract description 9
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- 230000006835 compression Effects 0.000 abstract description 2
- 238000007906 compression Methods 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- 239000000203 mixture Substances 0.000 description 8
- KHOZXYSECXUORA-UHFFFAOYSA-N dec-9-ynoic acid Chemical compound OC(=O)CCCCCCCC#C KHOZXYSECXUORA-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
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- 239000004566 building material Substances 0.000 description 1
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- 230000002035 prolonged effect Effects 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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Abstract
本发明公开了一种利用钢渣与赤泥制备的发泡陶瓷及其工艺,涉及发泡陶瓷技术领域,通过取β‑环糊精加入蒸馏水中,加入氢氧化钠溶液,再加入2‑丁氧基苯磺酰氯,得到中间体A,将中间体A和NaN3溶于N,N二甲基甲酰胺中,得到中间体B,取聚醚大单体溶于二氯甲烷,加入9‑癸炔酸;解决了现有的发泡陶瓷制品烧结后内部存在大量的真空或半真空状态的封闭气泡,造成耐火极限下降的问题;用高空间位阻官能团改性制备性能更加优异的促熔分子,通过点击化学反应实现了大分子的结合,使得分子显示出更好地保塌性能和流变性能,从而使发泡陶瓷具有更优异的力学性能,大幅度提升抗压性。
Description
技术领域
本发明涉及发泡陶瓷技术领域,具体涉及一种利用钢渣与赤泥制备的发泡陶瓷及其工艺。
背景技术
发泡陶瓷制品作为一种新型绿色建筑材料,其内部具有大量的封闭气泡,因此具有轻质、隔音、保温等优点,发泡陶瓷多采用矿石尾矿、陶瓷废渣等作为基料,有利于解决固废污染的问题,目前,发泡陶瓷几乎以硅酸盐玻璃相为主,玻璃相含量具体占80%以上。
但是现有的发泡陶瓷制品烧结后内部存在大量的真空或半真空状态的封闭气泡,当发泡陶瓷制品表面受到高温加热时,发泡陶瓷制品内的玻璃相和晶相产生的热应力扩展较快,易发生破裂,造成耐火极限下降,且发泡陶瓷表面受热冲击时也会产生表面剥落的现象,随着作用时间的增加,不断向内部扩展,最终导致其失去结构强度而无法正常使用。
发明内容
为了克服上述的技术问题,本发明的目的在于提供了一种利用钢渣与赤泥制备的发泡陶瓷及其工艺:
(1)取β-环糊精加入蒸馏水中,加入氢氧化钠溶液,再加入2-丁氧基苯磺酰氯,得到中间体A,将中间体A和NaN3溶于N,N二甲基甲酰胺中,得到中间体B,取聚醚大单体溶于二氯甲烷,加入9-癸炔酸,再加入4-二甲氨基吡啶,取N,N’-二环己基碳二亚胺加入CH2C l2溶液,得到N,N’-二环己基碳二亚胺溶液,并滴加到聚醚大单体溶液中,得到中间体C,将中间体B和中间体C溶于二甲基亚砜水溶液中,加入催化剂反应,得到该促熔助剂,解决了现有的发泡陶瓷制品烧结后内部存在大量的真空或半真空状态的封闭气泡,造成耐火极限下降的问题;
(2)将聚氧化丙烯二醇和三羟甲基丙烷聚乙二醇单甲醚置于三口烧瓶中,加入1,4-环己烷二异氰酸酯,得到中间体E,向含有中间体E的烧瓶中加入2,2-二羟甲基丙酸、异己二醇和丙酮,得到中间体F,向含有中间体F的烧瓶中加入催化剂,加入丙烯酸羟乙酯,得到中间体G,将中间体G转移至乳化桶中,加入三乙胺,并加入去离子水,得到该分散剂,解决了现有的发泡陶瓷制品表面受热冲击时,导致其失去结构强度而无法正常使用的问题。
本发明的目的可以通过以下技术方案实现:
一种利用钢渣与赤泥制备的发泡陶瓷,包括以下重量份组分:
钢渣20-30份、赤泥15-20份、二氧化硅30-40份、三氧化二铝10-50份、三氧化二铁2-6份、氧化钙2-5份、氧化钛1-2份、氧化钾1-6份、氧化钠2-3份、促熔助剂2-6份、分散剂2-4份、粘土5-7份;
该利用钢渣与赤泥制备的发泡陶瓷由以下步骤制备得到:
S1:将钢渣与二氧化硅、三氧化二铝、三氧化二铁、氧化钙、氧化钛、氧化钾和氧化钠混合均匀后浸泡于酸性溶液中,取出浸泡的原料干燥,得到陶瓷第一原料;
S2:将赤泥加入陶瓷第一原料中,并加入分散剂、促熔助剂和粘土,置于球磨罐中进行球磨,充分混合后,过筛再进行干燥,得到陶瓷第二原料;
S3:对陶瓷第二原料进行制粉、喷雾、造粒;
S4:对步骤S3所得到的产品进行烧结,制备得到利用钢渣与赤泥制备的发泡陶瓷。
作为本发明进一步的方案:所述促熔助剂由以下步骤制备得到:
S11:取β-环糊精加入蒸馏水中,在搅拌条件下加入氢氧化钠溶液,室温下搅拌,置于冰水浴中,再加入2-丁氧基苯磺酰氯在冰水浴条件下反应,过滤,在真空干燥箱中干燥,得到中间体A;
S12:将中间体A和NaN3溶于N,N二甲基甲酰胺中,在磁力搅拌条件下反应,得到中间体B;
S13:取聚醚大单体溶于二氯甲烷,加入9-癸炔酸,再加入4-二甲氨基吡啶,磁力搅拌,取N,N’-二环己基碳二亚胺加入CH2C l 2溶液,得到N,N’-二环己基碳二亚胺溶液,并滴加到聚醚大单体溶液中,控制滴加速度为1-2滴/s,室温条件下反应,得到中间体C;
S14:将中间体B和中间体C溶于二甲基亚砜水溶液中,加入催化剂反应,得到该促熔助剂。
作为本发明进一步的方案:步骤S11中所述β-环糊精、蒸馏水、氢氧化钠溶液与2-丁氧基苯磺酰氯的用量比为29g:300mL:150mL:24.9g,所述氢氧化钠溶液的浓度为1.8mol/L。
作为本发明进一步的方案:步骤S12中所述中间体A、NaN3、N,N二甲基甲酰胺的用量比为3.8g:1.3g:40mL。
作为本发明进一步的方案:步骤S13中所述聚醚大单体、二氯甲烷、9-癸炔酸、4-二甲氨基吡啶、N,N’-二环己基碳二亚胺与CH2C l2溶液的用量比为12g:60mL:16.8g:0.62g:1.85g:10mL。
作为本发明进一步的方案:步骤S14中所述中间体B与中间体C的用量比为1.9g:2.8g,所述催化剂为抗坏血酸钠,所述催化剂的用量为中间体B和中间体C总质量的3%,所述二甲基亚砜水溶液中二甲基亚砜与水的体积比为3:1。
作为本发明进一步的方案:所述分散剂由以下步骤制备得到:
S71:将聚氧化丙烯二醇和三羟甲基丙烷聚乙二醇单甲醚置于三口烧瓶中,并加装温度计、冷凝管、搅拌杆,然后真空脱水,冷却,加入1,4-环己烷二异氰酸酯,并通入干燥氮气保护,升温反应,冷却,得到中间体E;
S72:向含有中间体E的烧瓶中加入2,2-二羟甲基丙酸、异己二醇和丙酮,升温反应,冷却,得到中间体F;
S73:向含有中间体F的烧瓶中加入催化剂,升温反应,冷却,加入丙烯酸羟乙酯,冷却,得到中间体G;
S74:将中间体G转移至乳化桶中,加入三乙胺,并加入去离子水,高速剪切分散,得到该分散剂。
作为本发明进一步的方案:步骤S71中所述聚氧化丙烯二醇、三羟甲基丙烷聚乙二醇单甲醚和1,4-环己烷二异氰酸酯的用量比为40g:8.87g:28.55g,步骤S72中所述中间体E、2,2-二羟甲基丙酸、异己二醇与丙酮的用量比为78.69g:3.18g:5.67g:10mL。
作为本发明进一步的方案:步骤S73中所述催化剂为辛酸亚锡和二月桂酸二丁基锡按任意比例混合,所述催化剂的用量为中间体F质量的6%,所述中间体F与丙烯酸羟乙酯的用量比为87.65g:3.84g,步骤S74中所述中间体G、三乙胺与去离子水的用量比为81.54g:3.6mL:50mL。
一种利用钢渣与赤泥制备的发泡陶瓷的制备方法,包括以下步骤:
S1:将钢渣与二氧化硅、三氧化二铝、三氧化二铁、氧化钙、氧化钛、氧化钾和氧化钠混合均匀后浸泡于酸性溶液中,取出浸泡的原料干燥24-48h,得到陶瓷第一原料;
S2:将赤泥加入陶瓷第一原料中,并加入分散剂、促熔助剂和粘土,置于球磨罐中进行球磨2-4h,充分混合后,过筛再进行干燥5-10h,得到陶瓷第二原料;
S3:对陶瓷第二原料进行制粉、喷雾、造粒;
S4:对步骤S3所得到的产品进行烧结,制备得到利用钢渣与赤泥制备的发泡陶瓷。
本发明的有益效果:
(1)本发明是通过将聚氧化丙烯二醇和三羟甲基丙烷聚乙二醇单甲醚置于三口烧瓶中,加入1,4-环己烷二异氰酸酯,得到中间体E,向含有中间体E的烧瓶中加入2,2-二羟甲基丙酸、异己二醇和丙酮,得到中间体F,向含有中间体F的烧瓶中加入催化剂,加入丙烯酸羟乙酯,得到中间体G,将中间体G转移至乳化桶中,加入三乙胺,并加入去离子水,得到该分散剂,分散剂减小了模具模腔的摩擦力,使发泡陶瓷原料可以均匀地在模腔内流动,减小成形力,使生成的发泡陶瓷具有更高的力学性能,分散剂分子作用在发泡陶瓷原料之间,使得各成分分散均匀,在烧结过程中,大幅度减少真空状态和半真空状态的粉笔气泡,提高耐火极限;
(2)取β-环糊精加入蒸馏水中,加入氢氧化钠溶液,再加入2-丁氧基苯磺酰氯,得到中间体A,将中间体A和NaN3溶于N,N二甲基甲酰胺中,得到中间体B,取聚醚大单体溶于二氯甲烷,加入9-癸炔酸,再加入4-二甲氨基吡啶,取N,N’-二环己基碳二亚胺加入CH2C l2溶液,得到N,N’-二环己基碳二亚胺溶液,并滴加到聚醚大单体溶液中,得到中间体C,将中间体B和中间体C溶于二甲基亚砜水溶液中,加入催化剂反应,得到该促熔助剂,用高空间位阻官能团改性制备性能更加优异的促熔分子,通过点击化学反应实现了大分子的结合,制备了叠加两者空间位阻的促熔分子,成功地引入单烯烃双键,也通过自由基聚合反应将β-环糊精接枝在大分子的支链上,延长了侧链长度,提升了空间位阻效应,使得分子显示出更好地保塌性能和流变性能,从而使发泡陶瓷具有更优异的力学性能,大幅度提升抗压性。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1:
本实施例为一种利用钢渣与赤泥制备的发泡陶瓷,包括以下重量份组分:
钢渣20份、赤泥15份、二氧化硅30份、三氧化二铝10份、三氧化二铁2份、氧化钙2份、氧化钛1份、氧化钾1份、氧化钠2份、促熔助剂2份、分散剂2份、粘土5份;
该利用钢渣与赤泥制备的发泡陶瓷由以下步骤制备得到:
S1:将钢渣与二氧化硅、三氧化二铝、三氧化二铁、氧化钙、氧化钛、氧化钾和氧化钠混合均匀后浸泡于酸性溶液中12h,取出浸泡的原料干燥24h,得到陶瓷第一原料;
S2:将赤泥加入陶瓷第一原料中,并加入分散剂、促熔助剂和粘土,置于球磨罐中进行球磨2h,充分混合后,过筛再进行干燥5h,得到陶瓷第二原料;
S3:对陶瓷第二原料进行制粉、喷雾、造粒;
S4:对步骤S3所得到的产品进行烧结,制备得到利用钢渣与赤泥制备的发泡陶瓷;
所述促熔助剂由以下步骤制备得到:
S11:取29g的β-环糊精加入300mL的蒸馏水中,在搅拌条件下加入氢氧化钠溶液150mL,室温下搅拌5h,置于冰水浴中,温度控制在0℃,再加入24.9g的2-丁氧基苯磺酰氯在冰水浴条件下反应12h,过滤,在60℃的真空干燥箱中干燥10h,得到中间体A;
S12:将3.8g的中间体A和1.3gNaN3溶于40mL的N,N二甲基甲酰胺中,反应温度设定在80℃,在磁力搅拌条件下反应24h,得到中间体B;
S13:取12g的聚醚大单体溶于60mL的二氯甲烷,加入16.8g的9-癸炔酸,再加入0.62g的4-二甲氨基吡啶,磁力搅拌5mi n,取1.85g的N,N’-二环己基碳二亚胺加入10mL的CH2C l2溶液,得到N,N’-二环己基碳二亚胺溶液,并滴加到聚醚大单体溶液中,控制滴加速度为1滴/s,室温条件下反应24h,得到中间体C;
S14:将1.9g中间体B和2.8g中间体C溶于二甲基亚砜水溶液中,加入催化剂,80℃条件下反应30h,得到该促熔助剂;
所述分散剂由以下步骤制备得到:
S71:将聚氧化丙烯二醇和三羟甲基丙烷聚乙二醇单甲醚置于三口烧瓶中,并加装温度计、冷凝管、搅拌杆,然后在100℃下真空脱水60mi n,冷却至40℃,加入1,4-环己烷二异氰酸酯,并通入干燥氮气保护,升温至90℃反应3h,冷却至50℃以下,得到中间体E;
S72:向含有中间体E的烧瓶中加入2,2-二羟甲基丙酸、异己二醇和丙酮,升温至80℃反应1h,冷却至40℃,得到中间体F;
S73:向含有中间体F的烧瓶中加入辛酸亚锡和二月桂酸二丁基锡,升温至70℃反应3h,冷却至40℃,加入丙烯酸羟乙酯,反应2h,冷却至40℃,得到中间体G;
S74:将中间体G转移至乳化桶中,在1000r/mi n的转速下,加入三乙胺中和成盐,并加入去离子水,高速剪切分散10mi n,得到该分散剂。
实施例2:
本实施例为一种利用钢渣与赤泥制备的发泡陶瓷,包括以下重量份组分:
钢渣30份、赤泥15份、二氧化硅40份、三氧化二铝10份、三氧化二铁2份、氧化钙5份、氧化钛1份、氧化钾4份、氧化钠2份、促熔助剂2份、分散剂4份、粘土5份;
该利用钢渣与赤泥制备的发泡陶瓷由以下步骤制备得到:
S1:将钢渣与二氧化硅、三氧化二铝、三氧化二铁、氧化钙、氧化钛、氧化钾和氧化钠混合均匀后浸泡于酸性溶液中24h,取出浸泡的原料干燥48h,得到陶瓷第一原料;
S2:将赤泥加入陶瓷第一原料中,并加入分散剂、促熔助剂和粘土,置于球磨罐中进行球磨4h,充分混合后,过筛再进行干燥10h,得到陶瓷第二原料;
S3:对陶瓷第二原料进行制粉、喷雾、造粒;
S4:对步骤S3所得到的产品进行烧结,制备得到利用钢渣与赤泥制备的发泡陶瓷;
所述促熔助剂由以下步骤制备得到:
S11:取29g的β-环糊精加入300mL的蒸馏水中,在搅拌条件下加入氢氧化钠溶液150mL,室温下搅拌6h,置于冰水浴中,温度控制在5℃,再加入24.9g的2-丁氧基苯磺酰氯在冰水浴条件下反应24h,过滤,在70℃的真空干燥箱中干燥12h,得到中间体A;
S12:将3.8g的中间体A和1.3gNaN3溶于40mL的N,N二甲基甲酰胺中,反应温度设定在90℃,在磁力搅拌条件下反应26h,得到中间体B;
S13:取12g的聚醚大单体溶于60mL的二氯甲烷,加入16.8g的9-癸炔酸,再加入0.62g的4-二甲氨基吡啶,磁力搅拌10mi n,取1.85g的N,N’-二环己基碳二亚胺加入10mL的CH2C l2溶液,得到N,N’-二环己基碳二亚胺溶液,并滴加到聚醚大单体溶液中,控制滴加速度为1滴/s,室温条件下反应28h,得到中间体C;
S14:将1.9g中间体B和2.8g中间体C溶于二甲基亚砜水溶液中,加入催化剂,90℃条件下反应24h,得到该促熔助剂;
所述分散剂由以下步骤制备得到:
S71:将聚氧化丙烯二醇和三羟甲基丙烷聚乙二醇单甲醚置于三口烧瓶中,并加装温度计、冷凝管、搅拌杆,然后在100℃下真空脱水60mi n,冷却至40℃,加入1,4-环己烷二异氰酸酯,并通入干燥氮气保护,升温至90℃反应3h,冷却至50℃以下,得到中间体E;
S72:向含有中间体E的烧瓶中加入2,2-二羟甲基丙酸、异己二醇和丙酮,升温至80℃反应1h,冷却至40℃,得到中间体F;
S73:向含有中间体F的烧瓶中加入辛酸亚锡和二月桂酸二丁基锡,升温至70℃反应3h,冷却至40℃,加入丙烯酸羟乙酯,反应2h,冷却至40℃,得到中间体G;
S74:将中间体G转移至乳化桶中,在1000r/mi n的转速下,加入三乙胺中和成盐,并加入去离子水,高速剪切分散10mi n,得到该分散剂。
实施例3:
本实施例为一种利用钢渣与赤泥制备的发泡陶瓷,包括以下重量份组分:
钢渣20份、赤泥15份、二氧化硅30份、三氧化二铝30份、三氧化二铁2份、氧化钙5份、氧化钛1份、氧化钾6份、氧化钠3份、促熔助剂6份、分散剂4份、粘土7份;
该利用钢渣与赤泥制备的发泡陶瓷由以下步骤制备得到:
S1:将钢渣与二氧化硅、三氧化二铝、三氧化二铁、氧化钙、氧化钛、氧化钾和氧化钠混合均匀后浸泡于酸性溶液中24h,取出浸泡的原料干燥48h,得到陶瓷第一原料;
S2:将赤泥加入陶瓷第一原料中,并加入分散剂、促熔助剂和粘土,置于球磨罐中进行球磨4h,充分混合后,过筛再进行干燥10h,得到陶瓷第二原料;
S3:对陶瓷第二原料进行制粉、喷雾、造粒;
S4:对步骤S3所得到的产品进行烧结,制备得到利用钢渣与赤泥制备的发泡陶瓷;
所述促熔助剂由以下步骤制备得到:
S11:取29g的β-环糊精加入300mL的蒸馏水中,在搅拌条件下加入氢氧化钠溶液150mL,室温下搅拌6h,置于冰水浴中,温度控制在5℃,再加入24.9g的2-丁氧基苯磺酰氯在冰水浴条件下反应12h,过滤,在70℃的真空干燥箱中干燥10h,得到中间体A;
S12:将3.8g的中间体A和1.3gNaN3溶于40mL的N,N二甲基甲酰胺中,反应温度设定在80℃,在磁力搅拌条件下反应24h,得到中间体B;
S13:取12g的聚醚大单体溶于60mL的二氯甲烷,加入16.8g的9-癸炔酸,再加入0.62g的4-二甲氨基吡啶,磁力搅拌5mi n,取1.85g的N,N’-二环己基碳二亚胺加入10mL的CH2C l2溶液,得到N,N’-二环己基碳二亚胺溶液,并滴加到聚醚大单体溶液中,控制滴加速度为2滴/s,室温条件下反应28h,得到中间体C;
S14:将1.9g中间体B和2.8g中间体C溶于二甲基亚砜水溶液中,加入催化剂,90℃条件下反应30h,得到该促熔助剂;
所述分散剂由以下步骤制备得到:
S71:将聚氧化丙烯二醇和三羟甲基丙烷聚乙二醇单甲醚置于三口烧瓶中,并加装温度计、冷凝管、搅拌杆,然后在100℃下真空脱水60mi n,冷却至40℃,加入1,4-环己烷二异氰酸酯,并通入干燥氮气保护,升温至90℃反应3h,冷却至50℃以下,得到中间体E;
S72:向含有中间体E的烧瓶中加入2,2-二羟甲基丙酸、异己二醇和丙酮,升温至80℃反应1h,冷却至40℃,得到中间体F;
S73:向含有中间体F的烧瓶中加入辛酸亚锡和二月桂酸二丁基锡,升温至70℃反应3h,冷却至40℃,加入丙烯酸羟乙酯,反应2h,冷却至40℃,得到中间体G;
S74:将中间体G转移至乳化桶中,在1000r/mi n的转速下,加入三乙胺中和成盐,并加入去离子水,高速剪切分散10mi n,得到该分散剂。
对比例1:
对比例1与实施例1的不同之处在于不添加分散剂。
对比例2:
对比例2使用市购发泡陶瓷。
性能测试
将实施例1-3以及对比例1-2的发泡陶瓷进行检测;
检测结果如下表所示:
由上表可知,实施例的发泡均匀程度均为均匀,对比例1的发泡均匀程度也为均匀,对比例2的发泡均匀程度为上下层孔径不一致,实施例的吸水率为0.03-0.04%,对比例1的吸水率为0.15%,对比例2的吸水率为1.20%,实施例的烧成时间低于对比例1,对比例1的烧成时间又低于对比例2,实施例的实验效果均优于对比例,故该工艺生产的发泡陶瓷相较于现有技术性能得到大幅提高。
在本说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (10)
1.一种利用钢渣与赤泥制备的发泡陶瓷,其特征在于,包括以下重量份组分:
钢渣20-30份、赤泥15-20份、二氧化硅30-40份、三氧化二铝10-50份、三氧化二铁2-6份、氧化钙2-5份、氧化钛1-2份、氧化钾1-6份、氧化钠2-3份、促熔助剂2-6份、分散剂2-4份、粘土5-7份;
该利用钢渣与赤泥制备的发泡陶瓷由以下步骤制备得到:
S1:将钢渣与二氧化硅、三氧化二铝、三氧化二铁、氧化钙、氧化钛、氧化钾和氧化钠混合均匀后浸泡于酸性溶液中,取出浸泡的原料干燥,得到陶瓷第一原料;
S2:将赤泥加入陶瓷第一原料中,并加入分散剂、促熔助剂和粘土,置于球磨罐中进行球磨,过筛再进行干燥,得到陶瓷第二原料;
S3:对陶瓷第二原料进行制粉、喷雾、造粒;
S4:对步骤S3所得到的产品进行烧结,制备得到发泡陶瓷。
2.根据权利要求1所述的一种利用钢渣与赤泥制备的发泡陶瓷,其特征在于,所述促熔助剂由以下步骤制备得到:
S11:取β-环糊精加入蒸馏水中,在搅拌条件下加入氢氧化钠溶液,室温下搅拌,置于冰水浴中,再加入2-丁氧基苯磺酰氯在冰水浴条件下反应,过滤,在真空干燥箱中干燥,得到中间体A;
S12:将中间体A和NaN3溶于N,N二甲基甲酰胺中,在磁力搅拌条件下反应,得到中间体B;
S13:取聚醚大单体溶于二氯甲烷,加入9-癸炔酸,再加入4-二甲氨基吡啶,磁力搅拌,取N,N’-二环己基碳二亚胺加入CH2Cl2溶液,得到N,N’-二环己基碳二亚胺溶液,并滴加到聚醚大单体溶液中,控制滴加速度为1-2滴/s,室温条件下反应,得到中间体C;
S14:将中间体B和中间体C溶于二甲基亚砜水溶液中,加入催化剂反应,得到该促熔助剂。
3.根据权利要求2所述的一种利用钢渣与赤泥制备的发泡陶瓷,其特征在于,步骤S11中所述β-环糊精、蒸馏水、氢氧化钠溶液与2-丁氧基苯磺酰氯的用量比为29g:300mL:150mL:24.9g,所述氢氧化钠溶液的浓度为1.8mol/L。
4.根据权利要求2所述的一种利用钢渣与赤泥制备的发泡陶瓷,其特征在于,步骤S12中所述中间体A、NaN3、N,N二甲基甲酰胺的用量比为3.8g:1.3g:40mL。
5.根据权利要求2所述的一种利用钢渣与赤泥制备的发泡陶瓷,其特征在于,步骤S13中所述聚醚大单体、二氯甲烷、9-癸炔酸、4-二甲氨基吡啶、N,N’-二环己基碳二亚胺与CH2Cl2溶液的用量比为12g:60mL:16.8g:0.62g:1.85g:10mL。
6.根据权利要求2所述的一种利用钢渣与赤泥制备的发泡陶瓷,其特征在于,步骤S14中所述中间体B与中间体C的用量比为1.9g:2.8g,所述催化剂为抗坏血酸钠,所述催化剂的用量为中间体B和中间体C总质量的3%,所述二甲基亚砜水溶液中二甲基亚砜与水的体积比为3:1。
7.根据权利要求1所述的一种利用钢渣与赤泥制备的发泡陶瓷,其特征在于,所述分散剂由以下步骤制备得到:
S71:将聚氧化丙烯二醇和三羟甲基丙烷聚乙二醇单甲醚置于三口烧瓶中,并加装温度计、冷凝管、搅拌杆,然后真空脱水,冷却,加入1,4-环己烷二异氰酸酯,并通入干燥氮气保护,升温反应,冷却,得到中间体E;
S72:向含有中间体E的烧瓶中加入2,2-二羟甲基丙酸、异己二醇和丙酮,升温反应,冷却,得到中间体F;
S73:向含有中间体F的烧瓶中加入催化剂,升温反应,冷却,加入丙烯酸羟乙酯,冷却,得到中间体G;
S74:将中间体G转移至乳化桶中,加入三乙胺,并加入去离子水,高速剪切分散,得到该分散剂。
8.根据权利要求7所述的一种利用钢渣与赤泥制备的发泡陶瓷,其特征在于,步骤S71中所述聚氧化丙烯二醇、三羟甲基丙烷聚乙二醇单甲醚和1,4-环己烷二异氰酸酯的用量比为40g:8.87g:28.55g,步骤S72中所述中间体E、2,2-二羟甲基丙酸、异己二醇与丙酮的用量比为78.69g:3.18g:5.67g:10mL。
9.根据权利要求7所述的一种利用钢渣与赤泥制备的发泡陶瓷,其特征在于,步骤S73中所述催化剂为辛酸亚锡和二月桂酸二丁基锡按任意比例混合,所述催化剂的用量为中间体F质量的6%,所述中间体F与丙烯酸羟乙酯的用量比为87.65g:3.84g,步骤S74中所述中间体G、三乙胺与去离子水的用量比为81.54g:3.6mL:50mL。
10.根据权利要求1-9任一项所述的一种利用钢渣与赤泥制备的发泡陶瓷的制备方法,其特征在于,包括以下步骤:
S1:将钢渣与二氧化硅、三氧化二铝、三氧化二铁、氧化钙、氧化钛、氧化钾和氧化钠混合均匀后浸泡于酸性溶液中,干燥,得到陶瓷第一原料;
S2:将赤泥加入陶瓷第一原料中,并加入分散剂、促熔助剂和粘土,置于球磨罐中进行球磨,过筛再进行干燥,得到陶瓷第二原料;
S3:对陶瓷第二原料进行制粉、喷雾、造粒;
S4:对步骤S3所得到的产品进行烧结,制备得到发泡陶瓷。
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