CN113087610A - 对叔丁基苯甲酸制备系统 - Google Patents
对叔丁基苯甲酸制备系统 Download PDFInfo
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- KDVYCTOWXSLNNI-UHFFFAOYSA-N 4-t-Butylbenzoic acid Chemical compound CC(C)(C)C1=CC=C(C(O)=O)C=C1 KDVYCTOWXSLNNI-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- QCWXDVFBZVHKLV-UHFFFAOYSA-N 1-tert-butyl-4-methylbenzene Chemical compound CC1=CC=C(C(C)(C)C)C=C1 QCWXDVFBZVHKLV-UHFFFAOYSA-N 0.000 claims abstract description 45
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000012043 crude product Substances 0.000 claims abstract description 31
- 239000003054 catalyst Substances 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 17
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- 239000001301 oxygen Substances 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000000741 silica gel Substances 0.000 claims description 28
- 229910002027 silica gel Inorganic materials 0.000 claims description 28
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 26
- 229940011182 cobalt acetate Drugs 0.000 claims description 16
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 16
- 238000005804 alkylation reaction Methods 0.000 claims description 15
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 claims description 12
- 230000003213 activating effect Effects 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229940071125 manganese acetate Drugs 0.000 claims description 6
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 6
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 6
- 229940053662 nickel sulfate Drugs 0.000 claims description 6
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 229940075581 sodium bromide Drugs 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 4
- ZDFKSZDMHJHQHS-UHFFFAOYSA-N 2-tert-butylbenzoic acid Chemical compound CC(C)(C)C1=CC=CC=C1C(O)=O ZDFKSZDMHJHQHS-UHFFFAOYSA-N 0.000 claims 1
- 238000007670 refining Methods 0.000 claims 1
- 238000001816 cooling Methods 0.000 abstract description 12
- 238000005406 washing Methods 0.000 abstract description 8
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 238000001953 recrystallisation Methods 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- -1 polypropylene Polymers 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- AXHVNJGQOJFMHT-UHFFFAOYSA-N 1-tert-butyl-2-methylbenzene Chemical compound CC1=CC=CC=C1C(C)(C)C AXHVNJGQOJFMHT-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- QPJVMBTYPHYUOC-UHFFFAOYSA-N Methyl benzoate Natural products COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- FXXACINHVKSMDR-UHFFFAOYSA-N acetyl bromide Chemical compound CC(Br)=O FXXACINHVKSMDR-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000010730 cutting oil Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229940095102 methyl benzoate Drugs 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
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- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/255—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting
- C07C51/265—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting having alkyl side chains which are oxidised to carboxyl groups
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- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/08—Silica
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Abstract
本发明提供对叔丁基苯甲酸制备系统,包括如下步骤:步骤一,获得对叔丁基甲苯;步骤二,制备负载型复合催化剂;步骤三,步骤一中得到的对叔丁基甲苯和步骤二中负载型复合催化剂加入至反应釜中,通入氧气,在两个梯度温度下进行氧化反应,得到对叔丁基苯甲酸粗品;步骤四,将步骤三中得到的对叔丁基苯甲酸粗品进行降温析晶、离心甩干,用对叔丁基甲苯进行打洗,得到离心粗品;步骤五,将步骤四中的离心粗品加入到溶解釜中,加入甲苯升温溶解,转料至重结晶釜进行降温析晶,干燥后得到对叔丁基苯甲酸成品。本发明的有益效果是:本发明采用粗品经过简单的水洗即可得到高品质的产品,简化了后处理工艺,可提高产品的品质并降低生产成本。
Description
技术领域
本发明涉及对叔丁基苯甲酸制备领域,更具体地说涉及一种对叔丁基苯甲酸制备系统。
背景技术
对叔丁基苯甲酸是有机合成中间体,主要用于聚丙成核剂、聚氯乙烯热稳定剂、金属加工切削和润滑油的添加剂、抗氧剂、醇酸树脂改性剂、助焊剂及染料等多种特殊功能。
现有技术中在获得叔丁基甲苯后,将其与醋酸钴和溴化物组成的催化剂加入反应釜,升温并通入氧气,得到对叔丁基苯甲酸粗品,经活性炭、硅藻土脱色、结晶和干燥即得对叔丁基苯甲酸。但该方法用的催化剂为醋酸钴和溴化钠的复合催化剂,在生产过程中有溴化物存在,后处理难以处理;使用活性炭、硅藻土脱色,工艺步骤复杂,会对后续对叔丁基苯甲酸甲酯的生产带来麻烦。
发明内容
本发明克服了现有技术中的不足,提供了一种对叔丁基苯甲酸制备系统。
本发明的目的通过下述技术方案予以实现。
对叔丁基苯甲酸制备系统,包括如下步骤:
步骤一,获得对叔丁基甲苯;
步骤二,制备负载型复合催化剂,具体制备步骤为:将醋酸钴、醋酸锰、溴化钠、硫酸镍按摩尔比1∶3∶4∶0.5利用去离子水配置成混合溶液,在搅拌的条件下加入硅胶形成溶胶,并使所述硅胶恰好能与醋酸钴和溴化钠的混合溶液等体积浸渍;将溶胶在室温下静置陈化48h,然后在150℃下烘干溶胶,再于350℃下活化1.5h,最后在450℃下活化7h,制得负载型复合催化剂;
步骤三,所述步骤一中得到的所述对叔丁基甲苯和所述步骤二中负载型复合催化剂加入至反应釜中,通入氧气在两个梯度温度下进行氧化反应,得到对叔丁基苯甲酸粗品;
步骤四,将所述步骤三中得到的对叔丁基苯甲酸粗品进行降温析晶、离心甩干,用对叔丁基甲苯进行打洗,得到离心粗品;
步骤五,将所述步骤四中的离心粗品加入到溶解釜中,加入甲苯升温溶解,转料至重结晶釜进行降温析晶,干燥后得到对叔丁基苯甲酸成品。
优选地,所述步骤一中获得对叔丁基甲苯的具体方法为:
S1,将甲苯和浓硫酸加入到反应釜中,通入异丁烯进行烷基化反应,得到粗品对叔丁基甲苯;
S2,将所述第一步中获得的粗品对叔丁基甲苯进行精馏得到对叔丁基甲苯。
由上述任一方案优选的是,所述S1的烷基化反应的温度为20-24℃,时间为9-11小时。
由上述任一方案优选的是,所述步骤三中在所述反应釜中分为两个温度梯度进行氧化反应,第一反应梯度的温度为140-150℃,反应时间为2-3h;第二反应梯度的温度为120-135℃,反应时间为4-6小时。
由上述任一方案优选的是,所述步骤三中所述负载型复合催化剂的加入量是对叔丁基甲苯重量的0.1-1.0%。
由上述任一方案优选的是,所述硅胶的表面积为10-700m2/g。
由上述任一方案优选的是,所述硅胶的孔体积为0.1-4.0ml/g。
由上述任一方案优选的是,所述硅胶的平均粒径为0.1-500μm。
本发明的有益效果为:
传统采用醋酸作溶剂,醋酸钴作催化剂,高温,高压法制备对叔丁基苯甲酸;本发明以对叔丁基甲苯为原料,同时作为溶剂,其中加入复合催化剂,常压氧化法,降低了生产成本;
以醋酸钴为自制的负载型复合催化剂的一部分,通过优化反应条件和后处理过程,实现了在无溴化物存在下合成目标产物对叔丁基苯甲酸,避免了因溴化物的存在造成后处理复杂以及着色效应。此外,也避免了因溴化物的存在造成对设备的腐蚀;应用该自制的负载型复合催化剂,不再使用醋酸、溴化物等试剂,从而可消除这些试剂所造成的腐蚀以及后处理复杂的问题;
采用两段温度反应的方法,得到对叔丁基苯甲酸粗品,此法避免了因溴化物的存在而造成的设备腐蚀以及后处理复杂的问题。
本发明采用粗品经过简单的水洗即可得到高品质的产品,简化了后处理工艺,可提高产品的品质并降低生产成本,本发明从根本上改变了对叔丁基苯甲酸合成工艺复杂、产品纯度低的现状,解决了其作为重要的有机合成中间体面临的品质不高难题。
具体实施方式
下面通过具体的实施例对本发明的技术方案作进一步的说明。
对叔丁基苯甲酸制备系统,包括如下步骤:
步骤一,获得对叔丁基甲苯。所述步骤一中获得对叔丁基甲苯的具体方法为:
S1,将甲苯和浓硫酸加入到反应釜中,通入异丁烯进行烷基化反应,得到粗品对叔丁基甲苯;
S2,将所述第一步中获得的粗品对叔丁基甲苯进行精馏得到对叔丁基甲苯;
所述S1的烷基化反应的温度为20-24℃,时间为9-11小时。
步骤二,制备负载型复合催化剂,具体制备步骤为:将醋酸钴、醋酸锰、溴化钠、硫酸镍按摩尔比1∶3∶4∶0.5利用去离子水配置成混合溶液,在搅拌的条件下加入硅胶形成溶胶,并使所述硅胶恰好能与醋酸钴和溴化钠的混合溶液等体积浸渍;将溶胶在室温下静置陈化48h,然后在150℃下烘干溶胶,再于350℃下活化1.5h,最后在450℃下活化7h,制得负载型复合催化剂。
所述硅胶的表面积为10-700m2/g;所述硅胶的孔体积为0.1-4.0ml/g;所述硅胶的平均粒径为0.1-500μm。优选地,硅胶的表面积为10-700m2/g,更优选硅胶的表面积为50-500m2/g,最优选地硅胶的表面积为100-400m2/g;
硅胶的孔体积为0.1-4.0ml/g,更优选地硅胶的孔体积为0.5-3.5ml/g,最优选地硅胶的孔体积为0.8-3.0ml/g;
硅胶的平均粒径为0.1-500μm范围,硅胶的平均粒径更优选地为1-200μm,最优选地硅胶的平均粒径为10-100μm。
步骤三,所述步骤一中得到的所述对叔丁基甲苯和所述步骤二中负载型复合催化剂加入至反应釜中,通入氧气,在两个梯度温度下进行氧化反应,得到对叔丁基苯甲酸粗品;
所述步骤三中在所述反应釜中分为两个温度梯度进行氧化反应,首先在温度为140-150℃的条件下,反应2-3h,然后在温度为120-135℃的条件下,反应4-6h。
所述步骤三中所述负载型复合催化剂的加入量是对叔丁基甲苯重量的0.1-1.0%。
步骤四,将所述步骤三中得到的对叔丁基苯甲酸粗品进行降温析晶、离心甩干,用对叔丁基甲苯进行打洗,得到离心粗品;
步骤五,将所述步骤四中的离心粗品加入到溶解釜中,加入甲苯升温溶解,转料至重结晶釜进行降温析晶,干燥后得到对叔丁基苯甲酸成品。
实施例1
1、获得对叔丁基甲苯:将甲苯和浓硫酸加入到反应釜中,通入异丁烯进行烷基化反应,得到粗品对叔丁基甲苯,烷基化反应的温度为20℃,时间为11小时,然后将粗品对叔丁基甲苯进行精馏得到对叔丁基甲苯。
2、制备负载型复合催化剂,具体制备步骤为:将醋酸钴、醋酸锰、溴化钠、硫酸镍按摩尔比1∶3∶4∶0.5利用去离子水配置成混合溶液,在搅拌的条件下加入硅胶形成溶胶,并使所述硅胶恰好能与醋酸钴和溴化钠的混合溶液等体积浸渍;将溶胶在室温下静置陈化48h,然后在150℃下烘干溶胶,再于350℃下活化1.5h,最后在450℃下活化7h,制得负载型复合催化剂;
3、对叔丁基苯甲酸的合成反应:将对叔丁基甲苯和钛沸石、负载型催化剂加入到反应釜中,通入含90%氧气和其他惰性气体的气体混合物,在反应开始阶段,温度在140℃开始进行反应,并在该温度下进行氧化反应3h;然后将温度降低至120℃继续进行氧化反应,反应时间为4h,得到对叔丁基苯甲酸粗品。
4、对叔丁基苯甲酸粗品进行降温析晶、离心甩干,用对叔丁基甲苯进行打洗,得到离心粗品。
5、将所述步骤四中的离心粗品加入到溶解釜中,加入甲苯升温溶解,转料至重结晶釜进行降温析晶,干燥后得到对叔丁基苯甲酸成品。
由此制得的对叔丁基苯甲酸成品为白色结晶,无机械杂质,熔点范围介于165.0-166.1℃,酸值介于314-316mgKOH/g,HPLC检测纯度为99.5%,水分含量为0.07%,甲苯含量为0.06%。
实施例2
1、获得对叔丁基甲苯:将甲苯和浓硫酸加入到反应釜中,通入异丁烯进行烷基化反应,得到粗品对叔丁基甲苯,烷基化反应的温度为24℃,时间为9小时,然后将粗品对叔丁基甲苯进行精馏得到对叔丁基甲苯。
2、制备负载型复合催化剂,具体制备步骤为:将醋酸钴、醋酸锰、溴化钠、硫酸镍按摩尔比1∶3∶4∶0.5利用去离子水配置成混合溶液,在搅拌的条件下加入硅胶形成溶胶,并使所述硅胶恰好能与醋酸钴和溴化钠的混合溶液等体积浸渍;将溶胶在室温下静置陈化48h,然后在150℃下烘干溶胶,再于350℃下活化1.5h,最后在450℃下活化7h,制得负载型复合催化剂;
3、对叔丁基苯甲酸的合成反应:将对叔丁基甲苯和钛沸石、负载型催化剂加入到反应釜中,通入含90%氧气和其他惰性气体的气体混合物,在反应开始阶段,温度在150℃开始进行反应,并在该温度下进行氧化反应2h;然后将温度降低至135℃继续进行氧化反应,反应时间为6h,得到对叔丁基苯甲酸粗品。
4、对叔丁基苯甲酸粗品进行降温析晶、离心甩干,用对叔丁基甲苯进行打洗,得到离心粗品。
5、将所述步骤四中的离心粗品加入到溶解釜中,加入甲苯升温溶解,转料至重结晶釜进行降温析晶,干燥后得到对叔丁基苯甲酸成品。
由此制得的对叔丁基苯甲酸成品为白色结晶,无机械杂质,熔点范围介于165.2-166.3℃,酸值介于314-316mgKOH/g,HPLC检测纯度为99.3%,水分含量为0.06%,甲苯含量为0.05%。
实施例3
1、获得对叔丁基甲苯:将甲苯和浓硫酸加入到反应釜中,通入异丁烯进行烷基化反应,得到粗品对叔丁基甲苯,烷基化反应的温度为22℃,时间为10小时,然后将粗品对叔丁基甲苯进行精馏得到对叔丁基甲苯。
2、制备负载型复合催化剂,具体制备步骤为:将醋酸钴、醋酸锰、溴化钠、硫酸镍按摩尔比1∶3∶4∶0.5利用去离子水配置成混合溶液,在搅拌的条件下加入硅胶形成溶胶,并使所述硅胶恰好能与醋酸钴和溴化钠的混合溶液等体积浸渍;将溶胶在室温下静置陈化48h,然后在150℃下烘干溶胶,再于350℃下活化1.5h,最后在450℃下活化7h,制得负载型复合催化剂;
3、对叔丁基苯甲酸的合成反应:将对叔丁基甲苯和钛沸石、负载型催化剂加入到反应釜中,通入含90%氧气和其他惰性气体的气体混合物,在反应开始阶段,温度在145℃开始进行反应,并在该温度下进行氧化反应2.5h;然后将温度降低至130℃继续进行氧化反应,反应时间为5h,得到对叔丁基苯甲酸粗品。
4、对叔丁基苯甲酸粗品进行降温析晶、离心甩干,用对叔丁基甲苯进行打洗,得到离心粗品。
5、将所述步骤四中的离心粗品加入到溶解釜中,加入甲苯升温溶解,转料至重结晶釜进行降温析晶,干燥后得到对叔丁基苯甲酸成品。
由此制得的对叔丁基苯甲酸成品为白色结晶,无机械杂质,熔点范围介于164.5-166.5℃,酸值介于314-316mgKOH/g,HPLC检测纯度为99.4%,水分含量为0.07%,甲苯含量为0.04%。
以上对本发明的三个实施例进行了详细说明,但所述内容仅为本发明的较佳实施例,不能被认为用于限定本发明的实施范围。凡依本发明申请范围所作的均等变化与改进等,均应仍归属于本发明的专利涵盖范围之内。
Claims (7)
1.对叔丁基苯甲酸制备系统,其特征在于:包括如下步骤:
步骤一,获得对叔丁基甲苯;
步骤二,制备负载型复合催化剂,具体制备步骤为:将醋酸钴、醋酸锰、溴化钠、硫酸镍按摩尔比1∶3∶4∶0.5利用去离子水配置成混合溶液,在搅拌的条件下加入硅胶形成溶胶,并使所述硅胶恰好能与醋酸钴和溴化钠的混合溶液等体积浸渍;将溶胶在室温下静置陈化48h,然后在150℃下烘干溶胶,再于350℃下活化1.5h,最后在450℃下活化7h,制得负载型复合催化剂;
步骤三,所述步骤一中得到的所述对叔丁基甲苯和所述步骤二中负载型复合催化剂加入至反应釜中,通入氧气,在两个梯度温度下进行氧化反应,得到对叔丁基苯甲酸粗品;
所述步骤三中在所述反应釜中氧化反应的步骤为:首先在温度为140-150℃的条件下,反应2-3h,然后在温度为120-135℃的条件下,反应4-6h。
步骤四,将所述步骤三中得到的对叔丁基苯甲酸粗品进行离心粗品,在将离心粗品进行精化得到叔丁基苯甲酸成品。
2.根据权利要求1所述的对叔丁基苯甲酸制备系统,其特征在于:所述步骤一中获得对叔丁基甲苯的具体方法为:
S1,将甲苯和浓硫酸加入到反应釜中,通入异丁烯进行烷基化反应,得到粗品对叔丁基甲苯;
S2,将所述第一步中获得的粗品对叔丁基甲苯进行精馏得到对叔丁基甲苯。
3.根据权利要求2所述的对叔丁基苯甲酸制备系统,其特征在于:所述S1的烷基化反应的温度为20-24℃,时间为9-11小时。
4.根据权利要求3所述的对叔丁基苯甲酸制备系统,其特征在于:所述步骤三中所述负载型复合催化剂的加入量是对叔丁基甲苯重量的0.1-1.0%。
5.根据权利要求4所述的对叔丁基苯甲酸制备系统,其特征在于:所述硅胶的表面积为10-700m2/g。
6.根据权利要求5所述的对叔丁基苯甲酸制备系统,其特征在于:所述硅胶的孔体积为0.1-4.0ml/g。
7.根据权利要求6所述的对叔丁基苯甲酸制备系统,其特征在于:所述硅胶的平均粒径为0.1-500μm。
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