CN101177617B - 一种制备生物柴油的工艺方法 - Google Patents
一种制备生物柴油的工艺方法 Download PDFInfo
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- CN101177617B CN101177617B CN2006101144405A CN200610114440A CN101177617B CN 101177617 B CN101177617 B CN 101177617B CN 2006101144405 A CN2006101144405 A CN 2006101144405A CN 200610114440 A CN200610114440 A CN 200610114440A CN 101177617 B CN101177617 B CN 101177617B
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- methanol
- biofuel
- vegetables oil
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- 239000003225 biodiesel Substances 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000000463 material Substances 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 239000003054 catalyst Substances 0.000 claims abstract description 25
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerine Chemical compound 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OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 235000011187 glycerol Nutrition 0.000 claims abstract description 11
- 230000035484 reaction time Effects 0.000 claims abstract description 9
- 238000004062 sedimentation Methods 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 33
- 235000013311 vegetables Nutrition 0.000 claims description 29
- 239000002551 biofuel Substances 0.000 claims description 22
- 238000005809 transesterification reaction Methods 0.000 claims description 21
- 238000004821 distillation Methods 0.000 claims description 19
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- 108090000790 Enzymes Proteins 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound 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OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- WVDDGKGOMKODPV-UHFFFAOYSA-N benzyl alcohol Chemical compound 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OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 1
- 229960004217 benzyl alcohol Drugs 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000003197 catalytic Effects 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 230000002153 concerted Effects 0.000 description 1
- 230000001143 conditioned Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000002815 homogeneous catalyst Substances 0.000 description 1
- 238000011068 load Methods 0.000 description 1
- 230000001264 neutralization Effects 0.000 description 1
- 239000010773 plant oil Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
Abstract
本发明涉及一种制备生物柴油的工艺方法，用粗制植物油和工业甲醇为原料，采用复配碱催化剂进行酯交换反应，反应压力在0.2MPa～0.5MPa，反应温度在70℃～140℃，反应3～50分钟；反应后的物料经过沉降、闪蒸、减压精镏后处理工艺得到生物柴油产品。本发明的制备工艺方法能有效的提高酯交换反应的速度，缩短反应时间，不需要对原料进行精制，工艺简单，且反应条件温和，催化剂用量少，转化率高，后处理过程不会产生大量的废水。原料最好转化率达到99％，得到生物柴油的纯度、粘度、酸价、辛烷值、甘油含量和皂化值等都符合0#柴油的标准。
Description
一种制备生物柴油的工艺方法
技术领域
[0001] 本发明涉及一种采用酯交换法生产生物柴油的工艺方法，具体涉及以粗制植物油 和工业甲醇为原料，在碱催化下合成生物柴油的方法。
背景技术
[0002] 目前，生物 柴油主要用动植物油脂与一些短链烃（甲醇、乙醇等）在酸、碱催化、酶 催化或者超临界下发生酯交换反应的方法生产。
[0003] 传统的酯交换反应采用强酸、强碱均相催化剂，在常压、60°C左右（甲醇沸点温度 以下）的条件下进行反应，反应条件温和，但是反应时间往往需要1小时以上，油脂的转化 率才能达到95%。其中强酸作催化剂，由于反应速度慢，一般用于预处理原料中的自由脂 肪酸（FFA)；强碱作催化剂（如Na0H、K0H、甲醇钠等），用量约为(油重）左右，转化率 高，但同时也存在着显著的缺点，催化剂用量相对较多，产品需中和洗涤而带来大量的工业 废水，造成环境污染，后处理复杂。另外，采用上述传统强碱催化的酯交换反应生产生物柴 油时，为了保证原料的高转化率和催化剂有效利用，原料进入反应器前必须经过精制，以脱 除其中的水份和自由脂肪酸（FFA)，工艺步骤相对复杂。如专利（公开号：US2005/0081435 Al)中采用H2SO4为催化剂，H2SO4分别加入两个串联的连续搅拌反应釜（CSTR)中，在硫酸 的催化下先使FFA与甲醇发生酯化反应，原料甲醇需要经过干燥过程除去水分，然后进行 酯交换反应生成生物柴油。专利（公开号CN 1556174A)提到，高酸值动植物油酯首先与甘 油在强酸催化剂的存在下进行酯化，并采用共沸蒸馏溶剂。蒸出酯化反应生成的水分，进而 得到酯化混合物，酯化混合物与甲醇混合在强碱催化下进行酯交换反应。
[0004] 固体碱催化剂用于酯交换反应时，产品呈中性，无废水产生，催化剂可以多次重复 使用。但是反应速度慢，反应时间长达2小时以上（公开号：CN16640772A)，并且固体碱催 化剂需要负载、回收和活化。
[0005] 用超临界非催化法进行酯交换反应，反应快，时间短，转化率可达95 %以上，产品 不需要洗涤，后处理简单，但醇油摩尔比高，反应温度与压力超过甲醇的临界温度和临界压 力（一般在IOMPa〜30MPa、200°C〜350°C条件下)，生产工艺对设备要求高。
发明内容
[0006] 本发明目的就是克服上述制备方法的不足，提供一种能有效的提高用强碱作催化 剂酯交换反应的速度，缩短反应时间，不需要对原料进行精制，工艺简单，催化剂用量少，转 化率高，后处理过程产生的废水少的生物柴油制备方法。
[0007] 主要的技术方案：
[0008] 以粗制植物油和工业甲醇为原料，采用复配碱催化剂进行酯交换反应，反应压力 在0. 2MPa〜0. 5MPa，反应温度在70°C〜140°C，反应3〜40分钟；其中粗制植物油和工业 甲醇摩尔比为1 :4〜10，复配碱催化剂与粗制植物油质量比为0. 5〜1 ： 100，反应后的物 料经过沉降、闪蒸和/或减压精镏后处理工艺得到生物柴油产品；所述的复配碱催化剂由KOH、NaOH和Ca (OH) 2强碱复合而成，其中以摩尔比计，KOH =NaOH =Ca (OH) 2为95〜98 ： 1〜 4 :0· 5 〜1。
[0009] 上述粗制植物油和工业甲醇较优的摩尔比范围是1 :6〜7，甲醇用量少会降低粗 制植物油的转化率，而过大又会增加工艺运行费用；
[0010] 上述的复配碱催化剂与粗制植物油质量比应在所述的范围内选择，催化剂用量 大，反应速度快，但是同时增加了副反应。
[0011] 上述的复配碱催化剂与工业甲醇首先按比例掺混，形成甲醇/碱溶液后再与粗制 植物油混合进行酯交换反应。
[0012] 上述的反应条件温度、压力和时间根据不同的工艺过程控制，一般地时间增加或 者温度升高会导致副反应增加。优选的反应时间控制在3-10分钟，温度80°C -130°C。
[0013] 本发明的酯交换反应可以采用单个反应釜间歇操作工艺。反应釜内有搅拌装置，外有加热夹套。将掺混的甲醇/碱溶液与粗制植物油按照一定比例加入反应釜，控制升温 速率，使反应釜温度10〜40分钟升至100°C〜140°C，反应釜压力达到0. 3MPa〜0. 5MPa。 然后物料在搅拌下冷却至常温。把反应釜内的物料转入沉降器中静置0. 5〜3小时，混 合物分两层：下层为甘油层、上层为生物柴油层。将生物柴油层在60°C〜80°C，真空度 0. 0967MPa〜0. 0980MPa条件下进行常规的减压蒸馏出甲醇，再在200°C〜220°C下减压 蒸馏出生物柴油产品。上述连续操作时，更优的操作是10分钟将反应釜内温度逐步升至 130°C左右。时间增加或者温度升高会导致副反应增加。本单釜工艺也可以采用多个单釜 并联，通过控制各釜不同的进、出料顺序，作到连续出料。
[0014] 上述的酯交换反应优选采用多釜串连工艺连续操作。反应釜内带有搅拌装置，外 有加热夹套。甲醇/碱溶液与预热过的粗制植物油按照一定比例连续地加入第一个反应 釜，釜内温度70°C〜90°C，压力0. 2MPa〜0. 25MPa，物料停留时间为2〜10分钟。物料经 泵增压后连续送入第二个反应釜，釜内温度100°C〜120°C，压力0. 25MPa〜0. 3MPa，物料 停留时间为2〜10分钟。然后物料经泵增压后连续送入第三个反应釜，釜内温度128°C〜 140°C，压力0. 35MPa〜0. 5MPa，物料停留时间为2〜10分钟。出料冷却后进入沉降罐，底 层为粗甘油，上层经减压阀减压后进入闪蒸罐，甲醇从闪蒸罐顶部排出，闪蒸罐底部的粗生 物柴油进行减压蒸馏，减压蒸馏塔塔内真空度0. 0967MPa〜0. 0980MPa，塔底部出料为副产 品，顶部出料经水冷后即得到生物柴油。较优的连续操作条件是使三个反应釜温度等比例 逐渐增加，并且第三个反应釜的较优温度在130°C左右，温度低则油脂转化率下降而温度过 高又导致副反应增加；每个反应釜的停留时间控制在4分钟左右，时间短则油脂转化率低， 时间长则不仅副反应增加而且需要体积更大的反应釜。
[0015] 上述的酯交换反应优选采用管式反应器连续操作以强化反应过程。管式反应器为 一般套管式，内管走反应物料，管内装有静态混合器；外管通入水蒸汽。甲醇/碱溶液与粗 制植物油按照一定比例连续地加入预混混合器，混合均勻后经泵增压后在第一预热器中与 反应后的物料换热，紧接着进入第二预热器，温度升至120°C〜140°C，然后物料经泵增压 至0.4MPa〜O.SMPa后进入管式反应器。停留时间为3〜10分钟。管式反应器内温度控 制在130°C左右为佳。出料出料冷却后进入沉降罐，底层为粗甘油，上层经减压阀减压后进 入闪蒸罐，甲醇从闪蒸罐顶部排出，闪蒸罐底部的粗生物柴油进行减压蒸馏，减压蒸馏塔真 空度0. 0967MPa〜0. 0980MPa，塔底部出料为副产品，顶部出料经水冷后即得到生物柴油。[0016] 本发明采用连续操作时，可以将出料先预热原料，冷却后再进入沉降罐，以利用出 料余热。
[0017] 本发明的效果：
[0018] 1、本发明采用复配强碱催化剂，在一定温度、压力下进行酯交换反应，明显提高了 酯交换反应速度，缩短了反应时间，植物油的转化率高，尤其是采用先将催化剂与甲醇掺混 的工艺步骤，得到更优的效果，使得反应时间最短至3分钟，原料最好转化率达到99%，得 到生物柴油的纯度、粘度、酸价、辛烷值、甘油含量和皂化值等都符合0#柴油的标准。且反 应条件温和，对设备材质无特殊要求。
[0019] 2、原料直接用粗制植物油和工业甲醇均无需经过脱酸或者脱水等预处理过程，工 艺流程简单。 [0020] 3、本发明采用复配碱催化剂，实验证明产生协同催化效果，与减压蒸馏工艺配合， 使催化剂用量明显小于传统的均相反应中的碱催化剂用量，后处理中需要的水量降低，产 生的工业废水也大大减少。
[0021 ] 本发明中的工艺方法可以连续生产，从而适用工艺化生产。 附图说明
[0022] 附图1 ：本发明用于多釜串连工艺连续生产生物柴油的工艺流程示意图
[0023] 附图2 ：本发明用于管式反应器连续生产生物柴油的工艺流程示意图
具体实施方式：
[0024] 下面，结合实施例对本发明的实施方案进一步说明。但是，本发明不限于所列出的 实施例。还应包括对本发明所保护方案的其他任何公知的改变。
[0025] 实施例1 ：单釜间歇式操作合成生物柴油
[0026]首先取 4. 788kgK0H、0. 145kg NaOH 和 0. 067kg Ca (OH) 2 制备复配催化剂，5kg 复配 催化剂与209kg工业甲醇在带有搅拌装置的密封反应釜中掺混，然后装入IOOOkg粗制植物 油。在反应釜内的热电偶和压力仪表检测和调控下，调节反应釜搅拌器的转速，使反应釜温 度在10分钟内达到130°C，压力达到0. 4MPa，然后立即水冷至常温。把反应釜内的混合物 转入沉降器中静置120分钟，混合物分两层：下层为甘油层、上层为生物柴油层。将生物柴 油层在60°C，真空度0. 0967MPa条件下进行减压蒸馏除去甲醇，然后在220°C下继续减压蒸 馏即得到精制生物柴油产品。所得生物柴油产品得质量和性能测试结果如下：植物油转化 率99%，粘度9. 28mm2/S，和0#柴油相似，热值为40. 86MJ/kg，闪点192°C ；内燃机的性能测 试，表明生物柴油燃烧产生的动力良好，烟的浓度、CO和未燃碳氢化合物的排放降低，是一 种可替代的石化柴油的环境友好型替代燃料。对甘油层采用常规的分离方法处理残留催化 剂时，废水大量减少。
[0027] 实施例2 ：
[0028] 本实施例基于1，600kg/h处理量。主要参数见表1、表2，工艺流程如图1所示。
[0029] 按照实施例1的方法和比例复配催化剂，然后按催化剂与工业甲醇质量比2. 3 ： 100的比例配置甲醇/碱溶液，常温下，甲醇/碱溶液与预热到60°C的粗制植物油按照物质 的量的比6 :1的比例连续地加入带搅拌的反应釜1中，釜内温度88°C，压力0. 2MPa，物料停留时间为4分钟，植物油转化率达到39%。紧接着物料经泵2增压后连续送入带搅拌的反 应釜3，釜内温度110°C，压力0. 3MPa，物料停留时间为4. 3分钟，植物油转化率达到78%。 然后物料经泵4增压后连续送入带搅拌的反应釜5，釜内温度130°C，压力0. 4MPa,物料停留 时间为4. 5分钟，植物油转化率达到98%。反应后物料由泵6送入粗制柴油预热器7，利用 出料余热对粗制植物油预热，冷却后进入沉降罐8，底层为粗甘油，上层经减压阀9减压后 进入闪蒸罐10，甲醇从闪蒸罐顶部排出，闪蒸罐底部的粗生物柴油进入一个减压蒸馏塔11 进行减压蒸馏，减压蒸馏塔塔内真空度0. 0967MPa，塔底部出料为副产品，顶部出料经水冷 却器12冷却后就为最终产品——生物柴油。
[0030] 表1 ：实施例2的主要操作参数
[0031]
[0033] 表 2 ：实施例2的主要状态点参数 [0034]
[0035] 实施例3 ：
[0036] 本实施例基于1，600kg/h的处理量。工艺流程如图2所示。操作参数参数如表3、 表4、表5。
[0037] 按照实施例1的方法和比例复配催化剂，然后按实施例2中的比例配置甲醇/碱 溶液，常温下，甲醇/碱溶液与粗制植物油按照物质的量的比6 ：1的比例连续地加入预混 混合器13，混合均勻后物料经泵14增压至0. 3MPa后在第一预热器15中与反应后的物料 换热，温度升至70°C，紧接着进入第二预热器16，温度升至130°C，然后物料经泵17增压至 0.7MPa后进入管式反应器18。管内采用静态混合器强化传热。物料在反应器中停留时间 为3分钟，管式反应器出口植物油转化率达到99%。反应后物料进入第一预热器15，利用 出料余热预热原料，然后进入沉降罐19，底层为粗甘油，上层经泵20增加后再经减压阀21 减压后进入闪蒸罐22，甲醇从闪蒸罐顶部排出，闪蒸罐底部的粗生物柴油进入一个减压蒸馏塔23进行减压蒸馏，减压蒸馏塔塔内真空度约0. 0967MPa，塔底部出料为副产品，顶部出 料经水冷却器24冷却后就为最终产品——生物柴油。
[0038] 表3 ：实施例3的设备参数
[0039]
[0040] 表4 ：实施例3的操作参数
[0041]
[0042]表5：实施例3中各状态点参数[0043]
Claims (8)
- 一种制备生物柴油的工艺方法，用动植物油和工业甲醇，在碱催化下进行酯交换反应，其特征在于，用粗制植物油和工业甲醇为原料，采用复配碱催化剂进行酯交换反应，反应压力在0.2MPa～0.5MPa，反应温度在70℃～140℃，反应3～50分钟；其中粗制植物油和工业甲醇摩尔比为1∶4～10，复配的碱催化剂与粗制植物油质量比为0.5～1∶100，反应后的物料经过沉降、闪蒸和/或减压精镏后处理工艺得到生物柴油产品；所述的复配碱催化剂由KOH、NaOH和Ca(OH)2复配而成，其中以摩尔比计，KOH∶NaOH∶Ca(OH)2为95～98∶1～4∶0.5～1。
- 2.根据权利要求1所述的工艺方法，其特征在于：先将复配的碱催化剂与工业甲醇掺 混，形成甲醇/碱溶液后，再与其他原料混合进行酯交换反应。
- 3.根据权利要求1所述的方法，其特征在于：反应时间控制在3-10分钟，温度 800C -130°C。
- 4.根据权利要求1所述的工艺方法，其特征在于：酯交换反应采用单个反应釜操作，将 掺混的甲醇/碱溶液与粗制植物油按比例一同加入反应釜中，物料在不断搅拌下边升温边 反应，并控制升温速率，使得10〜40分钟后反应釜内温度逐步升至100°C〜140°C，反应釜 压力0. 3MPa〜0. 5MPa，然后物料在搅拌下冷却至常温，再转入沉降器沉降分层，将含生物 柴油的液体层经减压蒸馏得到甲醇和生物柴油产品。
- 5.根据权利要求4所述的工艺方法，其特征在于：将含生物柴油的液体层在60°C〜 80°C，真空度0. 0967MPa〜0. 0980MPa条件下进行减压蒸馏操作，除去甲醇后，再在200°C〜 220°C下继续减压蒸馏即得到精制生物柴油产品。
- 6.根据权利要求1所述的工艺方法，其特征在于：酯交换反应采用多釜串连工艺连续 操作，将配制的甲醇/碱溶液与预热过的粗制植物油按比例连续地加
- 7.根据权利要求1所述的工艺方法，其特征在于：酯交换反应采用管式反应器连续 操作以强化反应过程，管式反应器为套管式，内管走反应物料，管内装有静态混合器，外管 通入水蒸汽，甲醇/碱溶液与粗制植物油按配制比例连续地加入预混混合器，混合均勻后 物料经泵增压后在第一预热器中与反应后的物料换热，紧接着进入第二预热器，温度升至 120°C〜140°C，然后物料经泵增压至0. 4MPa〜0. 8MPa后进入管式反应器，停留时间为3〜 10分钟，出料冷却后进入沉降罐，底层为粗甘油，上层为含生物柴油的液体层，经减压阀减 压后进入闪蒸罐，甲醇从闪蒸罐顶部排出，闪蒸罐底部的粗生物柴油进行减压蒸馏，减压蒸 馏塔塔内真空度0. 0967MPa〜0. 0980MPa，塔底部出料为副产品，顶部出料经水冷后即得到 生物柴油。
- 8.根据权利要求6所述的工艺方法，其特征在于：反应出料先用于预热原料，冷却后再 进入沉降罐。
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| CN101624533B (zh) * | 2008-07-12 | 2014-04-16 | 程文波 | 一种生物柴油生产中酯交换反应方法及其装置 |
| CA2768717C (en) * | 2011-12-20 | 2021-03-02 | The Biofuel Partnership Limited | A biodiesel manufacturing system and apparatus |
| CN103060097B (zh) * | 2012-12-30 | 2014-11-26 | 上海油好同盟新能源科技有限公司 | 一种固体催化剂催化生产生物柴油连续化生产线 |
| CN104087426B (zh) * | 2014-06-06 | 2016-01-06 | 华南理工大学 | 一种节能环保型碱催化酯交换法生产生物柴油的装置及方法 |
| CN106833906A (zh) * | 2016-12-28 | 2017-06-13 | 山东金冠化工有限公司 | 地沟油连续釜式带压酯化降酸工艺 |
| CN107927536B (zh) * | 2017-12-01 | 2021-09-03 | 广州玉婷阁医药科技有限公司 | 含有二十八烷醇的保健品 |
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