CN106190451A - 一种醇醚硼酸酯型制动液的制备方法 - Google Patents
一种醇醚硼酸酯型制动液的制备方法 Download PDFInfo
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- CN106190451A CN106190451A CN201610475352.1A CN201610475352A CN106190451A CN 106190451 A CN106190451 A CN 106190451A CN 201610475352 A CN201610475352 A CN 201610475352A CN 106190451 A CN106190451 A CN 106190451A
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000012530 fluid Substances 0.000 title claims abstract description 47
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 19
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 28
- -1 ethylene glycol monobutyl ethers borate Chemical class 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 13
- DSILSMIQUPKHSH-UHFFFAOYSA-N 2-[2-(2-methoxyethoxy)ethoxy]ethoxyboronic acid Chemical compound COCCOCCOCCOB(O)O DSILSMIQUPKHSH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 7
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 7
- 238000005260 corrosion Methods 0.000 claims abstract description 6
- 230000007797 corrosion Effects 0.000 claims abstract description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 27
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 14
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 10
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 8
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 6
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 claims description 5
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical class CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 4
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 4
- 239000012964 benzotriazole Substances 0.000 claims description 4
- 229940106691 bisphenol a Drugs 0.000 claims description 4
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- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 239000004328 sodium tetraborate Substances 0.000 claims description 4
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- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical class CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 3
- 235000010288 sodium nitrite Nutrition 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- AKNUHUCEWALCOI-UHFFFAOYSA-N N-ethyldiethanolamine Chemical compound OCCN(CC)CCO AKNUHUCEWALCOI-UHFFFAOYSA-N 0.000 claims description 2
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- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
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- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 claims description 2
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 claims description 2
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 2
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
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- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 claims description 2
- WBHHMMIMDMUBKC-XLNAKTSKSA-N ricinelaidic acid Chemical compound CCCCCC[C@@H](O)C\C=C\CCCCCCCC(O)=O WBHHMMIMDMUBKC-XLNAKTSKSA-N 0.000 claims description 2
- 229960003656 ricinoleic acid Drugs 0.000 claims description 2
- FEUQNCSVHBHROZ-UHFFFAOYSA-N ricinoleic acid Natural products CCCCCCC(O[Si](C)(C)C)CC=CCCCCCCCC(=O)OC FEUQNCSVHBHROZ-UHFFFAOYSA-N 0.000 claims description 2
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 claims description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical group CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 150000003852 triazoles Chemical class 0.000 claims 1
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- 230000000052 comparative effect Effects 0.000 description 5
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- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical group CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- 101100191138 Arabidopsis thaliana DOT4 gene Proteins 0.000 description 2
- 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 description 2
- 101100427348 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) UBP10 gene Proteins 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- FUGIIBWTNARRSF-UHFFFAOYSA-N decane-5,6-diol Chemical compound CCCCC(O)C(O)CCCC FUGIIBWTNARRSF-UHFFFAOYSA-N 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical group CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
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- 230000008961 swelling Effects 0.000 description 2
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 2
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 1
- ATDANDYRMPPEPJ-UHFFFAOYSA-N 2-[2-(2-butoxyethoxy)ethoxy]ethoxyboronic acid Chemical compound CCCCOCCOCCOCCOB(O)O ATDANDYRMPPEPJ-UHFFFAOYSA-N 0.000 description 1
- WFSMVVDJSNMRAR-UHFFFAOYSA-N 2-[2-(2-ethoxyethoxy)ethoxy]ethanol Chemical compound CCOCCOCCOCCO WFSMVVDJSNMRAR-UHFFFAOYSA-N 0.000 description 1
- CNXNTBWVFVZNDI-UHFFFAOYSA-N C(C)(C)(C)OC(COCCOCCO)C Chemical compound C(C)(C)(C)OC(COCCOCCO)C CNXNTBWVFVZNDI-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 210000000080 chela (arthropods) Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 229960003511 macrogol Drugs 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- ZAOCWQZQPKGTRN-UHFFFAOYSA-N nitrous acid;sodium Chemical compound [Na].ON=O ZAOCWQZQPKGTRN-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
一种醇醚硼酸酯型制动液的制备方法，将以重量百分比计的以下原料投入到反应釜内，在室温至90℃的温度下，搅拌至各种原料充分溶解后，过滤，即可得到制动液产品，原料包括：三乙二醇单甲醚硼酸酯20～50％，数均分子量780的多乙二醇单丁醚硼酸酯10～45％，多乙二醇单烷基醚10‑40％，多甘醇10～40％，三乙二醇二甲醚0～15％，抗氧剂0～3％，pH值调节剂0～5％，缓蚀剂0～5％。本发明解决了常用的硼酸酯型制动液不稳定的问题，取得了以下优点：抗气阻能力强，低温流动性好，防锈，防腐蚀，对橡胶件适应性好，热稳定性优异。
Description
技术领域
本发明涉及制动液的制备方法，尤其涉及一种包括三乙二醇单甲醚硼酸酯和多乙二醇单丁醚硼酸酯的醇醚硼酸酯型制动液的制备方法。
背景技术
汽车制动液俗称刹车油，汽车制动器中加入制动液通过有名的帕斯卡原理：在向液体内施加压力时，液体在各方向上传递的压力相等。通过给汽车制动液施加压力，由主泵与分泵相互作用至制动泵活塞上，再施加到制动蹄(钳)，实现汽车制动。近二十年汽车工业快速发展，汽车制动系统的技术也极大提高，采用防抱死(ABS)和四轮制动电子平衡稳定系统(ESP)技术，都要求使用高温抗气阻能力强，低温条件下，制动响应时间更短，制动更灵活、更稳定的制动液，确保汽车行驶安全。
制动液主要由三大部分材料组成，第一部分是润滑基础液，它要有良好的润滑性，确保制动液系统中金属表面不易被破坏和活塞、皮碗不易损害。第二部分是稀释剂，它要保证高、低温黏度的适应性。最后是加入缓蚀剂，保证制动液和部件的使用寿命。
专利US 4204974中研制的含氮硼酸酯制动液中加入了甲基三乙二醇叔丁基醚，CN104611092A中加入了二乙二醇二丁醚，有效的调节了制动液的低温黏度。专利GB 1214171、US 3625899中加入了高浓度的硼酸酯，制备出抗气阻能力强的制动液。以上的专利及市场上的一些硼酸酯型制动液不同程度的存在着如下问题：选用的双烷基醚中含有叔丁醚或双丁基的醚，容水性差、橡胶膨胀性较大，制动液中的硼酸酯对水敏感，储存或吸水时、易析出沉淀物的难题，带来刹车不安全的隐患。为此，需要一种能够解决上述问题的硼酸酯型制动液。
发明内容
本发明的目的是要提供一种抗气阻性好，尤其是低温性能更优异， 防锈、防腐蚀性能、抗氧化、橡胶适应性、稳定性更好的醇醚硼酸酯型制动液的制备方法。
本发明的目的是通过以下技术方案实现的：提供一种醇醚硼酸酯型制动液的制备方法，所述制动液以重量百分比计，包括以下组分：三乙二醇单甲醚硼酸酯20～50％，数均分子量780的多乙二醇单丁醚硼酸酯10～45％，多乙二醇单烷基醚10-40％，多甘醇20～40％，三乙二醇二甲醚0～15％，抗氧剂0～3％，pH值调节剂0～5％，缓蚀剂0～5％；
所述制备方法包括：
将上述原料投入到反应釜内，在室温至90℃的温度下，搅拌至各种原料充分溶解后，过滤，即可得到制动液产品。
优选地，所述三乙二醇单甲醚硼酸酯的制备方法为：在有加热、减压蒸馏功能的密闭反应釜中，加入三乙二醇单甲醚，搅拌、升温至50℃时，将硼酸加入到反应釜内，搅拌、升温、负压(-0.06～-0.98MPa)，温度控制在80～160℃，反应4h。反应结束后，测定硼酸酯的平衡回流沸点大于280℃。得到合格的硼酸酯，即酯化完成。三乙二醇单甲醚与硼酸的摩尔比为3～4∶1。
优选地，所述三乙二醇单丁醚硼酸酯的制备方法为：在有加热、减压蒸馏功能的密闭反应釜中加入多乙二醇单丁醚，搅拌、升温至50℃时，将硼酸加入到反应釜内，搅拌、升温、负压(-0.06～-0.098MPa)，温度控制在80～160℃，反应4h。测定硼酸酯的平衡回流沸点大于280℃，得到合格的硼酸酯，即酯化完成。多乙二醇单丁醚和硼酸的摩尔比为3～4∶1。
所述制动液制备方法中的温度优选为30-80℃，更优选50-80℃。
所述多乙二醇单烷基醚优选为分子式RO(CH2CH2O)nH所示的多乙二醇单烷基醚的至少一种，其中
R为1至6个碳原子的烷基，优选为CH3、CH3CH2、CH3CHCH3、CH3CH2CH2CH2，n为2及以上的整数，优选为2、3、4。
所述多乙二醇单烷基醚为二乙二醇单甲醚、二乙二醇单乙醚、二乙二醇单丁醚、三乙二醇单甲醚、数均分子量为230的多乙二醇单甲醚、数均分子量为258.8的多乙二醇单丁醚、数均分子量为213.2的多乙二醇单 乙醚的至少一种
所述多甘醇优选为结构式为HO(CH2CH2O)nH所表示的多甘醇的至少一种，其中，
n：为2以上的整数，优选2、3、4。
或者，所述多甘醇优选为数均分子量为P-188、P-200、P-300的聚乙二醇的至少一种。
其中，三乙二醇二甲醚的含量优选为0.5～15％，优选2％-13％，更优选5-10％。
所述抗氧剂优选为双酚A、T501型抗氧剂的至少一种，含量优选为0.01％～2％，更优选0.1％～0.4％。
所述缓蚀剂优选为甲基苯骈三氮唑、苯骈三氮唑、硼砂、亚硝酸钠、油酸、蓖麻酸中的至少一种，含量优选为0.01％～5％。
所述pH值调节剂优选为二正丁胺、三正丁胺、甲基二乙醇胺、乙基二乙醇胺、丁胺醚、甲丙胺醚、乙丙胺醚、甲氧乙丙胺醚、硼砂中的一种或两种至少一种，含量优选为0.1％～5％。
本发明的有益效果：
在所述制动液中，硼酸酯、多乙二醇烷基醚和三乙二醇二甲醚对橡胶皮碗起到膨胀作用，多甘醇对橡胶皮碗起到收缩作用。本发明的技术在于平衡这两种作用，保证橡胶皮碗的膨胀大小满足FMVSS NO.116和GB12981-2012的要求。特别是本发明中加入的三乙二醇二甲醚，还起到降低低温运动黏度的特殊作用。
采用本发明方法制备出的硼酸酯制动液，具有优良的理化性能，该制动液的平衡回流沸点＞250℃，湿平衡回流沸点＞160℃，-40℃运动粘度＜1500。本发明制备的制动液具有低温流动性好，高温抗气阻性强，各项性能指标满足国标GB 12981-2012中的HZY4指标和美国FMVSS NO.116DOT4的质量要求。
具体实施方式
下面通过具体实施例对本发明进行具体描述。
实施例1
在1.2m3的调和釜中，加入三乙二醇单甲醚硼酸酯360公斤、多乙二醇单丁醚硼酸酯250公斤，三乙二醇单甲醚200公斤，二甘醇180公斤、抗氧剂T501 2公斤、甲基苯骈三氮唑1公斤，丁胺醚7公斤，将上述原料依次加入到反应釜中，在30℃下，搅拌30min，原料充分溶解后，过滤至成品罐中。
实施例2
在1.2m3的调和釜中，加入三乙二醇单甲醚硼酸酯400公斤、多乙二醇单丁醚硼酸酯200公斤，三乙二醇单乙醚150公斤，三乙二醇二甲醚60公斤、三甘醇180公斤、抗氧剂T5012公斤、苯骈三氮唑2公斤，甲丙胺醚6公斤，将上述原料依次加入到反应釜中，在50℃，搅拌60min，原料充分溶解后，过滤至成品罐中。
实施例3
在1.2m3的调和釜中，加入三乙二醇单甲醚硼酸酯430公斤、多乙二醇单丁醚硼酸酯120公斤，三乙二醇单甲醚200公斤，三乙二醇二甲醚80公斤、PEG-188 160公斤、双酚A 2公斤、苯骈三氮唑1公斤，丁胺醚7公斤，将上述原料依次加入到反应釜中，在80℃，常压搅拌120min，原料充分溶解后，过滤至成品罐中。
对比例1：
在GB 1214171中，按下列质量百分比：三乙二醇单甲醚硼酸酯为67.39％，三乙二醇单甲醚为23.20％，聚乙二醇300(数均分子量为300)7.62％，二乙醇胺为1.78％，亚硝酸钠为0.01％。
对比例2：
在CN 104611092A中，按下列质量百分比：三乙二醇单甲醚硼酸酯为61％，二乙二醇二丁醚为20.1％，四甘醇17％，双酚A为0.3％，亚硝酸钠为0.6％，乙醇胺为1.0％
本发明实施例制备的醇醚硼酸酯型制动液，均满足GB 12981-2012中HZY4和美国FMVSS NO.116中的DOT4质量规格的要求，与对比例的结果见表1。
表1醇醚硼酸酯型制动液的技术参数
※参照US 3972822中，蒸发的剩余物，放置在室温，观察产生沉淀物的时间长短，判定制动液的热稳定性。不产生沉淀物的硼酸酯型制动液，稳定性好。
从上表对比例1中，蒸发试验后剩余物，室温下放置3天，产生较多沉淀，同时对比例1的-40℃运动黏度大于1500mm2/s，对有色金属铜的腐蚀性较大，不符合GB 12981-2012的标准值。对比例2中，由于加入了二乙二醇二丁醚，导致橡胶膨胀性较大，当吸收一定量水时出现了白色浑浊物。
实施例中的试验结果表明：本发明的硼酸酯型制动液各项理化指标均超出DOT4、HZY4的质量要求。尤其是蒸发试验后，没有析出沉淀物，试验前、后的PH值变化很小，显示出本发明的硼酸酯型制动液稳定性好。特别是实施例3的理化指标达到制动液国标中HZY6和国际标准ISO 4925-2005中的Class 6的要求。
本发明并不意味着被说明书实施例的描述所局限，在没有脱离设计宗旨及其原理的前提下可以有所变化。上述实施例仅为本发明的较佳实施例之一，并非以此限制本发明的实施范围，故凡依本发明的形状、结构、原理所做的等效变化，均应涵盖于本发明的保护范围之内。
Claims (9)
1.一种醇醚硼酸酯型制动液的制备方法，所述制动液以重量百分比计，包括以下组分：
三乙二醇单甲醚硼酸酯20～50％，数均分子量780的多乙二醇单丁醚硼酸酯10-45％，多乙二醇单烷基醚10～40％，多甘醇10～40％，三乙二醇二甲醚0～15％，抗氧剂0～3％，pH值调节剂0～5％，缓蚀剂0～5％；
所述制备方法包括：
将上述原料投入到反应釜内，在室温至90℃的温度下，搅拌至各种原料充分溶解后，过滤，即可得到制动液产品。
2.如权利要求1所述的醇醚硼酸酯型制动液的制备方法，其中所述多乙二醇单烷基醚为分子式RO(CH2CH2O)nH所示的多乙二醇单烷基醚的至少一种，其中R为1至6个碳原子的烷基，优选为CH3、CH3CH2、CH3CHCH3、CH3CH2CH2CH2，n为2及以上的整数，优选2、3、4。
3.如权利要求1所述的醇醚硼酸酯型制动液的制备方法，其中所述多甘醇为结构式HO(CH2CH2O)nH所表示的多甘醇的至少一种，其中，
n为2以上的整数，优选2、3、4。
4.如权利要求1所述的醇醚硼酸酯型制动液的制备方法，其中所述多甘醇为数均分子量为P-188、P-200、P-300的聚乙二醇的至少一种，所述多乙二醇单烷基醚为二乙二醇单甲醚、二乙二醇单乙醚、二乙二醇单丁醚、三乙二醇单甲醚、数均分子量为230的多乙二醇单甲醚、数均分子量为258.8的多乙二醇单丁醚、数均分子量为213.2的多乙二醇单乙醚的至少一种。
5.如权利要求1所述的醇醚硼酸酯型制动液的制备方法，其中三乙二醇二甲醚的含量为0.5～15％，优选2-13％，更优选5-10％。
6.如权利要求1所述的醇醚硼酸酯型制动液的制备方法，其中所述抗氧剂为双酚A、T501型抗氧剂的至少一种，含量为0.1％～0.4％。
7.如权利要求1所述的醇醚硼酸酯型制动液的制备方法，其中所述缓蚀剂为甲基苯骈三氮唑、苯骈三氮唑、硼砂、亚硝酸钠、油酸、蓖麻酸中的至少一种，含量为0.01％～5％。
8.如权利要求1所述的醇醚硼酸酯型制动液的制备方法，其中所述pH值调节剂为二正丁胺、三正丁胺、甲基二乙醇胺、乙基二乙醇胺、丁胺醚、甲丙胺醚、乙丙胺醚、甲氧乙丙胺醚、硼砂的至少一种，含量为0.1％～5％。
9.如权利要求1所述的醇醚硼酸酯型制动液的制备方法，其中所述温度为30℃至80℃，优选50℃至80℃。
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| CN108048166A (zh) * | 2017-12-26 | 2018-05-18 | 湖北回天新材料股份有限公司 | 一种机动车辆制动液 |
| CN111518124A (zh) * | 2020-06-03 | 2020-08-11 | 辽宁大学 | 醇醚型硼酸酯润滑油添加剂及其制备方法和应用 |
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| CN108048166A (zh) * | 2017-12-26 | 2018-05-18 | 湖北回天新材料股份有限公司 | 一种机动车辆制动液 |
| CN111518124A (zh) * | 2020-06-03 | 2020-08-11 | 辽宁大学 | 醇醚型硼酸酯润滑油添加剂及其制备方法和应用 |
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| CN116042290A (zh) * | 2022-09-29 | 2023-05-02 | 上海本牧实业有限公司 | 一种阻燃稳定的硼酸酯制动液及其制备方法 |
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Application publication date: 20161207 |