CN114181757B - 一种磷酸酯抗燃油 - Google Patents
一种磷酸酯抗燃油 Download PDFInfo
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- CN114181757B CN114181757B CN202010961468.2A CN202010961468A CN114181757B CN 114181757 B CN114181757 B CN 114181757B CN 202010961468 A CN202010961468 A CN 202010961468A CN 114181757 B CN114181757 B CN 114181757B
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- phosphate
- tert
- fire
- resistant oil
- butyl
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- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 83
- 239000010452 phosphate Substances 0.000 title claims abstract description 83
- 230000009970 fire resistant effect Effects 0.000 title claims abstract description 70
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 51
- -1 tri-tert-butyl phenyl Chemical group 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims abstract description 18
- KHLAZQIVJFSQDS-UHFFFAOYSA-N tert-butyl diphenyl phosphate Chemical compound C=1C=CC=CC=1OP(=O)(OC(C)(C)C)OC1=CC=CC=C1 KHLAZQIVJFSQDS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 9
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 9
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 9
- 238000005260 corrosion Methods 0.000 claims abstract description 9
- 230000007797 corrosion Effects 0.000 claims abstract description 9
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 9
- 239000003112 inhibitor Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 28
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 10
- 229920001577 copolymer Polymers 0.000 claims description 10
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 10
- XQVWYOYUZDUNRW-UHFFFAOYSA-N N-Phenyl-1-naphthylamine Chemical compound C=1C=CC2=CC=CC=C2C=1NC1=CC=CC=C1 XQVWYOYUZDUNRW-UHFFFAOYSA-N 0.000 claims description 8
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 8
- 229920000570 polyether Polymers 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 7
- 238000007872 degassing Methods 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- VMZVBRIIHDRYGK-UHFFFAOYSA-N 2,6-ditert-butyl-4-[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 VMZVBRIIHDRYGK-UHFFFAOYSA-N 0.000 claims description 6
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 6
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 6
- 239000012964 benzotriazole Substances 0.000 claims description 6
- 150000001565 benzotriazoles Chemical class 0.000 claims description 6
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- CMGDVUCDZOBDNL-UHFFFAOYSA-N 4-methyl-2h-benzotriazole Chemical compound CC1=CC=CC2=NNN=C12 CMGDVUCDZOBDNL-UHFFFAOYSA-N 0.000 claims description 5
- 150000002924 oxiranes Chemical class 0.000 claims description 5
- SZIMYNVBPPNTMU-UHFFFAOYSA-N tert-butyl phenyl hydrogen phosphate Chemical compound CC(C)(C)OP(O)(=O)OC1=CC=CC=C1 SZIMYNVBPPNTMU-UHFFFAOYSA-N 0.000 claims description 5
- VLLMWSRANPNYQX-UHFFFAOYSA-N thiadiazole Chemical compound C1=CSN=N1.C1=CSN=N1 VLLMWSRANPNYQX-UHFFFAOYSA-N 0.000 claims description 5
- 150000004867 thiadiazoles Chemical class 0.000 claims description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 4
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 3
- DKCPKDPYUFEZCP-UHFFFAOYSA-N 2,6-di-tert-butylphenol Chemical compound CC(C)(C)C1=CC=CC(C(C)(C)C)=C1O DKCPKDPYUFEZCP-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 239000007859 condensation product Substances 0.000 claims 1
- 238000004043 dyeing Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 239000003921 oil Substances 0.000 abstract description 68
- 238000002360 preparation method Methods 0.000 abstract description 13
- 230000003647 oxidation Effects 0.000 abstract description 9
- 238000007254 oxidation reaction Methods 0.000 abstract description 9
- 230000002195 synergetic effect Effects 0.000 abstract description 6
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 239000010720 hydraulic oil Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 24
- MXWLJBLIKWUVIO-UHFFFAOYSA-N (2,3,4-tritert-butylphenyl) dihydrogen phosphate Chemical compound CC(C)(C)C1=CC=C(OP(O)(O)=O)C(C(C)(C)C)=C1C(C)(C)C MXWLJBLIKWUVIO-UHFFFAOYSA-N 0.000 description 8
- 230000003301 hydrolyzing effect Effects 0.000 description 6
- 239000013618 particulate matter Substances 0.000 description 6
- 238000010998 test method Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 230000002269 spontaneous effect Effects 0.000 description 3
- MDWVSAYEQPLWMX-UHFFFAOYSA-N 4,4'-Methylenebis(2,6-di-tert-butylphenol) Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 MDWVSAYEQPLWMX-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- YTSACTNRGUJEGO-UHFFFAOYSA-N oxirane prop-1-ene Chemical group CC=C.C1CO1 YTSACTNRGUJEGO-UHFFFAOYSA-N 0.000 description 2
- 231100000241 scar Toxicity 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- PWPCOFJMPGZUEH-UHFFFAOYSA-N CCC.C1CO1 Chemical compound CCC.C1CO1 PWPCOFJMPGZUEH-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- YICSVBJRVMLQNS-UHFFFAOYSA-N dibutyl phenyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OC1=CC=CC=C1 YICSVBJRVMLQNS-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002462 imidazolines Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种磷酸酯抗燃油,可广泛用于电力、机械、化工、能源、材料等领域,尤其适合用作机械设备的抗燃液压油。本发明提供的磷酸酯抗燃油,由以下组分的原料制备而成:磷酸叔丁基苯二苯酯、磷酸三叔丁基苯酯、磷酸三苯酯、抗氧剂、腐蚀抑制剂、抗乳化剂、抗泡剂。本发明涉及的磷酸酯抗燃油,各组分之间协同作用,从而使得本产品具有难以点燃和自熄灭的特点,同时还具有优异的氧化安定性、热稳定性、水解安定性和良好的润滑性,是一种安全长寿命综合性能优异的抗燃液压油。其制备工艺简单,反应条件温和,原料易得,产率高。
Description
技术领域
本发明涉及一种磷酸酯抗燃油,可广泛用于电力、机械、化工、能源、材料等领域,尤其适合用作机械设备的抗燃液压油。
背景技术
随着电力工业的发展,高参数(高温、高压)大容量(300MW及以上)的汽轮机发电机组日益得到广泛应用。过热蒸汽已达到540℃以上,超临界机组的蒸汽温度甚至达到了600℃。汽轮机调节系统大多靠近过热蒸汽管道,而且系统油压最高可达到14.5MPa以上,如果采用矿物油(自然点只有350℃左右)作为调节系统的液压工作介质,一旦发生油泄露现象,发生火灾的危险性极大。
磷酸酯抗燃油是一种合成油,与矿物油相比,它具有自燃点高,不易燃和自熄灭等特点。应用于汽轮机电液调节系统,可以大幅降低因油泄漏而引起火灾的危险性,对保障设备安全运行具有重要的意义。
发明内容
本发的目的在于提供一种磷酸酯抗燃油,该磷酸酯抗燃油具有难以点燃和自熄灭的特点,同时还具有优异的氧化安定性、热稳定性、水解安定性和良好的润滑性。
本发的另一目的在于提供该磷酸酯抗燃油的制备方法。
根据本发明的第一个方面,提供了一种磷酸酯抗燃油,由以下组分的原料制备而成:磷酸叔丁基苯二苯酯、磷酸三叔丁基苯酯、磷酸三苯酯、抗氧剂、腐蚀抑制剂、抗乳化剂、抗泡剂。
根据本发明第二方面,按照第一个方面的磷酸酯抗燃油,按质量百分比计,由以下组分的原料制备而成:磷酸叔丁基苯二苯酯50~85份、磷酸三叔丁基苯酯6~48.87份、磷酸三苯酯1~5份、抗氧剂0.1~1份、腐蚀抑制剂0.01~1份、抗乳化剂0.01~1份、抗泡剂0.01~1份。
作为上述技术方案的优选,所述的抗氧剂为2,6-二叔丁基对甲酚、4,4’-亚甲基双(2,6二叔丁基酚)、2,6-二叔丁基-α-二甲氨基对甲酚、N,N’-二异辛基二苯胺、N-苯基-α-萘胺的一种或几种组合。
作为上述技术方案的优选,所述的腐蚀抑制剂为苯三唑、甲基苯三唑、苯三唑衍生物、噻二唑、噻二唑衍生物的一种或几种组合。
作为上述技术方案的优选,所述的抗乳化剂为胺与环氧化物缩合物、环氧乙烷丙烷嵌段聚醚、聚环氧乙烷-环氧丙烷醚的一种或几种组合。
作为上述技术方案的优选,所述的抗泡剂为甲基硅油、丙烯酸与醚共聚物的一种或几种组合。
一种磷酸酯抗燃油的制备方法,包括以下步骤:
(1)将磷酸叔丁基苯二苯酯、磷酸三叔丁基苯酯、磷酸三苯酯依次加入反应釜,加入适量吸附剂,开启搅拌,控制搅拌速度为200~300r/min,控制反应釜内温度为65~75℃,搅拌60min。
(2)开启真空泵,控制反应釜内压力为-0.01~-0.04MPa,继续搅拌,脱气120min。
(3)用板框过滤器进行粗滤,滤液泵入调和釜,开启调和釜搅拌器,依次加入抗氧剂、腐蚀抑制剂、抗乳化剂、抗泡剂。
(4)用精密过滤器过滤到颗粒污染度为5级以下,制得磷酸酯抗燃油。
有益的技术效果
本发明涉及的磷酸酯抗燃油,各组分之间协同作用,从而使得本产品具有难以点燃和自熄灭的特点,同时还具有优异的氧化安定性、热稳定性、水解安定性和良好的润滑性,是一种安全长寿命综合性能优异的抗燃液压油。其制备工艺简单,反应条件温和,原料易得,产率高。
具体实施方式
实施例1:
一种磷酸酯抗燃油,按质量百分比计,由以下组分的原料制备而成:磷酸叔丁基苯二苯酯50份、磷酸三叔丁基苯酯48.87份、磷酸三苯酯1份、2,6-二叔丁基对甲酚0.1份、苯三唑0.01份、胺与环氧化物缩合物0.01份、甲基硅油0.01份。
其制备方法如下:
(1)将磷酸叔丁基苯二苯酯50份、磷酸三叔丁基苯酯48.87份、磷酸三苯酯1份依次加入反应釜,加入吸附剂,开启搅拌,控制搅拌速度为200~300r/min,控制反应釜内温度为65~75℃,搅拌60min。
(2)开启真空泵,控制反应釜内压力为-0.01~-0.04MPa,继续搅拌,脱气120min。
(3)用板框过滤器进行粗滤,滤液泵入调和釜,开启调和釜搅拌器,依次加入2,6-二叔丁基对甲酚0.1份、苯三唑0.01份、胺与环氧化物缩合物0.01份、甲基硅油0.01份。
(4)用精密过滤器过滤到颗粒污染度为5级以下,制得磷酸酯抗燃油。
实施例2:
一种磷酸酯抗燃油,按质量百分比计,由以下组分的原料制备而成:磷酸叔丁基苯二苯酯85份、磷酸三叔丁基苯酯6份、磷酸三苯酯5份、4,4’-亚甲基双(2,6二叔丁基酚)1份、甲基苯三唑1份、环氧化物缩合物1份、丙烯酸与醚共聚物1份。
其制备方法如下:
(1)将磷酸叔丁基苯二苯酯85份、磷酸三叔丁基苯酯6份、磷酸三苯酯5份依次加入反应釜,加入吸附剂,开启搅拌,控制搅拌速度为200~300r/min,控制反应釜内温度为65~75℃,搅拌60min
(2)开启真空泵,控制反应釜内压力为-0.01~-0.04MPa,继续搅拌,脱气120min。
(3)用板框过滤器进行粗滤,滤液泵入调和釜,开启调和釜搅拌器,依次加入4,4’-亚甲基双(2,6二叔丁基酚)1份、甲基苯三唑1份、环氧化物缩合物1份、丙烯酸与醚共聚物1份。
(4)用精密过滤器过滤到颗粒污染度为5级以下,制得磷酸酯抗燃油。
实施例3:
一种磷酸酯抗燃油,按质量百分比计,由以下组分的原料制备而成:磷酸叔丁基苯二苯酯65份、磷酸三叔丁基苯酯30份、磷酸三苯酯4份、2,6-二叔丁基-α-二甲氨基对甲酚0.2份、苯三唑衍生物0.4份、环氧乙烷丙烷嵌段聚醚0.3份、甲基硅油以及丙烯酸与醚共聚物0.1份。
其制备方法如下:
(1)将磷酸叔丁基苯二苯酯65份、磷酸三叔丁基苯酯30份、磷酸三苯酯4份依次加入反应釜,加入吸附剂,开启搅拌,控制搅拌速度为200~300r/min,控制反应釜内温度为65~75℃,搅拌60min。
(2)开启真空泵,控制反应釜内压力为-0.01~-0.04MPa,继续搅拌,脱气120min。
(3)用板框过滤器进行粗滤,滤液泵入调和釜,开启调和釜搅拌器,依次加入2,6-二叔丁基-α-二甲氨基对甲酚0.2份、苯三唑衍生物0.4份、环氧乙烷丙烷嵌段聚醚0.3份、甲基硅油以及丙烯酸与醚共聚物0.1份。
(4)用精密过滤器过滤到颗粒污染度为5级以下,制得磷酸酯抗燃油。
实施例4:
一种磷酸酯抗燃油,按质量百分比计,由以下组分的原料制备而成:磷酸叔丁基苯二苯酯72份、磷酸三叔丁基苯酯23份、磷酸三苯酯3.5份、N,N’-二异辛基二苯胺与N-苯基-α-萘胺0.2份、噻二唑与噻二唑衍生物0.8份、环氧乙烷丙烷嵌段聚醚与聚环氧乙烷-环氧丙烷醚0.3份、甲基硅油以及丙烯酸与醚共聚物0.2份。
其制备方法如下:
(1)将磷酸叔丁基苯二苯酯72份、磷酸三叔丁基苯酯23份、磷酸三苯酯3.5份依次加入反应釜,加入吸附剂,开启搅拌,控制搅拌速度为200~300r/min,控制反应釜内温度为65~75℃,搅拌60min。
(2)开启真空泵,控制反应釜内压力为-0.01~-0.04MPa,继续搅拌,脱气120min。
(3)用板框过滤器进行粗滤,滤液泵入调和釜,开启调和釜搅拌器,依次加入N,N’-二异辛基二苯胺与N-苯基-α-萘胺0.2份、噻二唑与噻二唑衍生物0.8份、环氧乙烷丙烷嵌段聚醚与聚环氧乙烷-环氧丙烷醚0.3份、甲基硅油以及丙烯酸与醚共聚物0.2份。
(4)用精密过滤器过滤到颗粒污染度为5级以下,制得磷酸酯抗燃油。
实施例5:
一种磷酸酯抗燃油,按质量百分比计,由以下组分的原料制备而成:磷酸叔丁基苯二苯酯80份、磷酸三叔丁基苯酯16份、磷酸三苯酯3.2份、2,6-二叔丁基对甲酚与2,6-二叔丁基-α-二甲氨基对甲酚0.4份、苯三唑与苯三唑衍生物0.2份、胺与环氧化物缩合物以及环氧乙烷丙烷嵌段聚醚0.1份、甲基硅油以及丙烯酸与醚共聚物0.1份。
其制备方法如下:
(1)将磷酸叔丁基苯二苯酯80份、磷酸三叔丁基苯酯16份、磷酸三苯酯3.2份依次加入反应釜,加入吸附剂,开启搅拌,控制搅拌速度为200~300r/min,控制反应釜内温度为65~75℃,搅拌60min。
(2)开启真空泵,控制反应釜内压力为-0.01~-0.04MPa,继续搅拌,脱气120min。
(3)用板框过滤器进行粗滤,滤液泵入调和釜,开启调和釜搅拌器,依次加入2,6-二叔丁基对甲酚与2,6-二叔丁基-α-二甲氨基对甲酚0.4份、苯三唑与苯三唑衍生物0.2份、胺与环氧化物缩合物以及环氧乙烷丙烷嵌段聚醚0.1份、甲基硅油以及丙烯酸与醚共聚物0.1份。
(4)用精密过滤器过滤到颗粒污染度为5级以下,制得磷酸酯抗燃油。
对照例1:
在实施例1的基础上,加入5份的磷酸三丁酯,制备方法同实施例1。
对照例2:
在实施例2基础上,将甲基苯三唑1份去除,制备方法同实施例2。
对照例3:
在实施例4的基础上,以咪唑啉衍生物代替噻二唑与噻二唑衍生物,制备方法同实施例4。
对照例4:
在实施例5的基础上,以磷酸二丁基苯基酯代替磷酸三苯酯,制备方法同实施例5。
性能测试:
1电厂用磷酸酯抗燃油的抗燃性
按照GB T 3536的试验方法,检测实施例及对照例中制得的磷酸酯抗燃油的闪点。按照DL/T 706的试验方法,检测实施例及对照例中制得的磷酸酯抗燃油的自燃点。结果列于表1。
表1磷酸酯抗燃油的闪点和自燃点
闪点(开口),℃ | 自燃点,℃ | |
DL/T 571质量标准 | ≥240 | ≥530 |
实施例1 | 252 | 541 |
实施例2 | 255 | 545 |
实施例3 | 256 | 548 |
实施例4 | 252 | 542 |
实施例5 | 258 | 550 |
对照例1 | 226 | 464 |
对照例2 | 251 | 543 |
对照例3 | 253 | 543 |
对照例4 | 243 | 535 |
结果显示,实施例1~5中制得的磷酸酯抗燃油的闪点和自燃点均高于DL/T571中新磷酸酯抗燃油的质量标准,具有良好的抗燃性。而对照例1中制得的磷酸酯抗燃油的闪点和自燃点不能够达到DL/T 571中新磷酸酯抗燃油的质量标准,而对照例4中制得的磷酸酯抗燃油的闪点和自燃点虽然能够达到DL/T 571中新磷酸酯抗燃油的质量标准,但性能不如实施例。由此可以看出,实施例中制得的磷酸酯抗燃油各磷酸酯组分之间的具有明显协同作用,改变磷酸酯组分会明显降低磷酸酯抗燃油的抗燃性能。
2磷酸酯抗燃油的氧化安定性
按照EN 14832的试验方法,检测实施例及对照例中制得的磷酸酯抗燃油的氧化安定性,结果列于表2。
表2磷酸酯抗燃油的氧化安定性
结果显示,实施例1~5中制得的磷酸酯抗燃油的氧化安定性试验各项指标均远优于DL/T 571中新磷酸酯抗燃油的质量标准,具有优异的氧化安定性。而对照例1不能满足DL/T 571的质量要求,对照例2~3虽然也可以满足DL/T 571的质量要求,但性能明显不如实施例。由此可以看出,实施例中制得的磷酸酯抗燃油各组分之间具有协同作用,改变其组分将明显降低磷酸酯抗燃油的氧化安定性。
3磷酸酯抗燃油的水解安定性
按照EN 14833的试验方法,检测实施例及对照例中制得的磷酸酯抗燃油的水解安定性,结果列于表3。
表3电厂用磷酸酯抗燃油的水解安定性
结果显示,实施例1~5中制得的磷酸酯抗燃油的水解安定性试验指标远优于DL/T571中新磷酸酯抗燃油的质量标准,具有优异的水解安定性。而对照例1不能满足DL/T 571的质量要求,对照例4虽然可以满足DL/T 571的质量要求,但性能不如实施例。由此可以看出,实施例中制得的磷酸酯抗燃油各磷酸酯组分之间的具有明显协同作用,改变磷酸酯组分会明显降低磷酸酯抗燃油的水解安定性能。
4磷酸酯抗燃油的润滑性
按照GB/T 3142的试验方法,检测实施例及对照例中制得的磷酸酯抗燃油的最大无卡咬负荷(PB)和烧结负荷(PD),执行SHT 0189,检测实施例中制得的磷酸酯抗燃油的磨斑直径(D)。结果列于表4。
表4磷酸酯抗燃油的最大无卡咬负荷(PB)、烧结负荷(PD)和磨斑直径(D)
最大无卡咬负荷(P<sub>B</sub>),N | 烧结负荷(P<sub>D</sub>),N | 磨斑直径(D),mm | |
实施例1 | 647 | 1568 | 0.527 |
实施例2 | 647 | 1568 | 0.521 |
实施例3 | 647 | 1568 | 0.516 |
实施例4 | 647 | 1568 | 0.520 |
实施例5 | 647 | 1568 | 0.531 |
对照例1 | 549 | 1235 | 0.612 |
对照例2 | 647 | 1568 | 0.511 |
对照例3 | 647 | 1568 | 0.523 |
对照例4 | 549 | 1235 | 0.603 |
结果显示,实施例1~5中制得的磷酸酯抗燃油的具有良好的润滑性。而对照例1和4中的磷酸酯抗燃油的润滑性能则明显实施例差。由此可以看出,实施例中制得的磷酸酯抗燃油各磷酸酯组分之间的具有明显协同作用,改变磷酸酯组分会明显降低磷酸酯抗燃油的润滑性能。
以上实施例仅为说明本发明的技术思想,不能以此限定本发明的保护范围,凡是按照本发明提出的技术思想,在技术方案基础上所做的任何改动,均落入本发明保护范围之内;本发明未涉及的技术均可通过现有技术加以实现。
Claims (2)
1.一种磷酸酯抗燃油,由以下组分的原料制备而成:磷酸叔丁基苯二苯酯、磷酸三叔丁基苯酯、磷酸三苯酯、抗氧剂、腐蚀抑制剂、抗乳化剂、抗泡剂;
磷酸叔丁基苯二苯酯50~85份、磷酸三叔丁基苯酯6~48.87份、磷酸三苯酯1~5份、抗氧剂0.1~1份、腐蚀抑制剂0.01~1份、抗乳化剂0.01~1份、抗泡剂0.01~1份;
所述的抗氧剂为2,6-二叔丁基对甲酚、4,4’-亚甲基双(2,6二叔丁基酚)、2,6-二叔丁基-α-二甲氨基对甲酚、N,N’-二异辛基二苯胺、N-苯基-α-萘胺的一种或几种组合;
所述的腐蚀抑制剂为苯三唑、甲基苯三唑、苯三唑衍生物、噻二唑、噻二唑衍生物的一种或几种组合;
所述的抗乳化剂为胺与环氧化物缩合物、环氧乙烷丙烷嵌段聚醚、聚环氧乙烷-环氧丙烷醚的一种或几种组合;
所述的抗泡剂为甲基硅油、丙烯酸与醚共聚物的一种或几种组合。
2.一种制备权利要求1中所述的磷酸酯抗燃油的方法,其步骤如下:
(1)将磷酸叔丁基苯二苯酯、磷酸三叔丁基苯酯、磷酸三苯酯依次加入反应釜,加入适量吸附剂,开启搅拌,控制搅拌速度为200~300r/min,控制反应釜内温度为65~75℃,搅拌60min;
(2)开启真空泵,控制反应釜内压力为-0.01--0.04MPa,继续搅拌,脱气120min;
(3)用板框过滤器进行粗滤,滤液泵入调和釜,开启调和釜搅拌器,依次加入抗氧剂、腐蚀抑制剂、抗乳化剂、抗泡剂;
(4)用精密过滤器过滤到颗粒无染度为5级以下,制得电厂用磷酸酯抗燃油。
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